Dissertations / Theses: 'Toxicología forense'

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Allendes, Pérez Christian. "Procesos analíticos de detección de productos fitosanitarios en toxicología postmortem." Tesis, Universidad de Chile, 2012. http://www.repositorio.uchile.cl/handle/2250/113428.

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Magister en Bioquímica área de especialización en Toxicología
No autorizada por el autor para ser publicada a texto completo en el Portal de Tesis Electrónicas.
Un gran número de intoxicaciones agudas letales se producen en el país debido al uso indebido de métodos químicos para el control de plagas. Sin embargo, no se encuentran implementados protocolos confiables para establecer el diagnóstico de intoxicaciones agudas producidas por agentes de control de plagas como los fitosanitarios, que contribuyan a brindar información a los tribunales de justicia para establecer la etiología tóxica. En respuesta a lo anteriormente descrito, en el presente trabajo se implementaron protocolos analíticos para la investigación de productos fitosanitarios en muestras biológicas postmortem. Se establecieron protocolos y se implementaron metodologías analíticas para la determinación cualitativa o cuantitativa de un grupo de pesticidas organofosforados (paration, metil paration y diazinon) y del tipo carbamatos (carbaril, methomil y aldicarb) en muestras ingresadas en el departamento de laboratorios del Instituto Médico Legal de Santiago de Chile, y procedentes del departamento de Tanatología. Las metodologías analíticas se basaron en un pre-tratamiento de las muestras de acuerdo a su naturaleza, extracción en fase sólida (SPE) y análisis cromatográfico con detectores de nitrógeno-fósforo (GC-NPD) y de espectrometría de masas (GC-MS). Estas metodologías fueron validadas y favorablemente comparadas en su eficiencia con respecto a aquellas existentes en el servicio. Este nuevo pre-tratamiento, asociado ahora con SPE, permitió obtener muy buenos resultados tras la aplicación de cromatografía en placa fina (TLC) con derivatización post-cromatografica, para identificar pesticidas organofosforados en contenido gástrico y carbamicos en sangre y contenido gástrico. Al mismo tiempo se implementó un método analítico adecuado para la cuantificación de pesticidas organofosforados en la matriz sangre (paration, metilparation y diazinon), mediante la aplicación de SPE y GC-NPD. Se obtuvieron las curvas de calibración para determinar los pesticidas organofosforados en la matriz sangre, en el intervalo de concentraciones comprendido entre 0,1 y 4,0 mg/L, lográndose coeficientes de determinación superiores a 0,99 para los tres pesticidas organofosforados. Los limites de detección (LOD) y cuantificación (LOQ) obtenidos con esta metodología se encuentran entre 0,05-0,06 mg/L y 0,17-0,19 mg/L respectivamente. Estos valores son adecuados de acuerdo a las concentraciones que se logran obtener en sangre luego de una intoxicación aguda por pesticidas, según la experiencia forense mundial. La recuperación de los pesticidas organofosforados desde las muestras de sangre fue superior o igual al 95%, con valores de repetibilidad menores o iguales a 6,5%, indicando un bajo grado de dispersión para el método. Al mismo tiempo se evaluó la precisión intermedia obteniéndose valores inferiores o iguales a 6,9% (RSD), siendo menores al máximo de 15% establecido como límite. Los parámetros de calidad del método analítico desarrollado se enmarcan dentro de los valores aceptados para una metodología destinada al análisis de muestras de sangre del tipo post-mortem, avalados por literatura internacional. La importancia del desarrollo e implementación de esta metodología de trabajo para el Servicio Médico Legal tiene un alto impacto debido a que se trata de los compuestos (pesticidas organofosforados y carbamicos) que estadísticamente se presentan con mayor frecuencia en las causas de muerte por intoxicación aguda por pesticidas (IAP). En consecuencia, esta metodología será una valiosa contribución al informe tanatológico final que debe presentar el médico ante los tribunales de justicia, cuando se encuentra frente a un caso por muerte por intoxicación por pesticidas.
A great number of lethal acute intoxications take place in the country due to the undue use of chemical methods for the control of plagues. However, reliable protocols are not implemented to establish the diagnosis of acute intoxications taken place by agents of control of plagues, as the phytosanitary, that contribute to offer information to the tribunals of justice to establish the toxic etiology. In answer to these facts, in this work were implemented analytical protocols for the investigation of products phytosanitary in biological postmortem samples. It were established and implemented analytical methodologies for the qualitative or quantitative detection of a group of organophosphorus pesticides (parathion, parathion methyl and diazinon) and carbamates (carbaril, methomil and aldicarb) in samples entered in the department of laboratories of the Legal Medical Institute of Santiago from Chile, and coming from the department of Tanatology. The analytical methodologies were based on a pre-treatment of the samples according to their nature, solid phase extraction and chromatographic analysis with nitrogen-phosphorus (GC-NPD) and mass spectrometry detectors (GC_MS). These methodologies were validated and favorably compared in their efficiency with regard to those existent ones in the service. This new sample treatment, associate now with SPE, allowed to obtain very good results after the application of thin layer chromatography (TLC) with postchromatographic derivatization, to identify organophosphorus pesticides in gastric content and carbamates in blood and gastric content. At the same time a suitable analytical method for the quantification of organophosphorus pesticides in blood samples was implemented (parathion, metilparathion and diazinon), by means of the application of SPE and GC-NPD. The calibration curves for determining the organophosphorus pesticides in blood samples were obtained between 0.1 and 4.0 mg/L, with coefficients of determination higher than 0.99 for the three organophosphorus pesticides. The limit of detection (LOD) and quantification (LOQ) obtained with this methodology ranged 0.05-0.06 mg/L and 0.17-0.19 mg/L, respectively. These values are adequate taking into account the concentrations reached in blood after an acute poisoning by pesticides, according to world-wide forensic experience. The recovery of the organophosphorus pesticides from the blood samples was higher or equal than 95% with values of repeatability lower or equal than 6.5% indicating a low degree of dispersion for the method. At the same time the intermediate precision showed values lower or equal than 6.9% (RSD), being lower than the maximum of 15% establishes as the limit. The quality parameters of the analytical method developed are within the ranges of acceptance for a methodology aimed to the analysis of blood samples of the type post-mortem examination, and are warranted by international literature. The importance of the development and implementation of this methodology of work for Legal Medical Service has a high impact because it is the compounds (organophosphorus and carbamates pesticides) that statistically appear most frequently in the death causes by acute poisoning by (IAP). As a consequence, this methodology will be a valuable contribution to the report that it must present the doctor before the justice courts, when as opposed to a case by death by poisoning by pesticides.

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Kulikoff, Bravo Aleida Naara. "Implementación de un sistema informático para gestión de base de datos, en el Laboratorio de Toxicología del Servicio Médico Legal." Tesis, Universidad de Chile, 2004. http://www.repositorio.uchile.cl/handle/2250/105411.

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Brancoli, Daniel Luz 1986. "O efeito da ivermectina na duração das fases de decomposição, sobre os insetos necrófagos e interpretação termográfica da distribuição espacial da massa larval de dípteros em carcaças de cabras (Capra aegragrus hircus L.,1758)." [s.n.], 2013. http://repositorio.unicamp.br/jspui/handle/REPOSIP/317460.

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Orientador: Arício Xavier Linhares
Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Biologia
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Resumo: A estimativa do intervalo pós-morte (IPM), período entre a ocorrência da morte e o momento em que o corpo ou carcaça é encontrado, é uma das principais utilizações de insetos na área forense. A partir de informações sobre a biologia, ecologia e distribuição geográfica dos insetos, bem como do comportamento de toda fauna presente em um corpo é possível estimar o menor intervalo da ocorrência da morte. Diversos fatores tais como temperatura, umidade, presença de substâncias tóxicas nos tecidos de uma carcaça, podem interferir no ciclo de vida de um inseto, afetando diretamente a estimativa do IPM quando esta é baseada em parâmetros biológicos do inseto. Por isso, múltiplos fatores devem ser considerados para que a perícia seja mais precisa. Com o aumento no número de mortes de animais de importância econômica devido à intoxicação medicamentosa, se faz necessárias pesquisas voltadas para a entomotoxicologia, uma área que carece de estudos específicos. Assim, o presente trabalho visou identificar a entomofauna associada a carcaças de cabras (Capra aegagrus hircus L.) mortas após tratamento com ivermectina, expostas em ambiente natural, além de averiguar possíveis diferenças na atratividade, no desenvolvimento dos imaturos que utilizaram esse substrato para alimentação e se a temperatura e o padrão de colonização da massa larval divergem entre as carcaças de animais mortos por intoxicação. Esse último parâmetro foi avaliado por meio de registros termográficos realizados em intervalos de 12 horas. Além da importância de fatores abióticos como luminosidade, temperatura, umidade e pluviosidade, pôde-se observar a ação da ivermectina nas carcaças tratadas, interferindo na composição da fauna colonizadora, no tempo total e em cada estágio da decomposição, assim como no padrão físico e comportamental das massas larvais em comparação ao grupo controle. Ainda foi demonstrado que a termografia pode ser utilizada como uma nova ferramenta em estudos periciais, auxiliando de forma significativa a avaliação dos parâmetros das massas larvais
Abstract: The estimation of the postmortem interval (PMI), period between the occurrence of death and the time at which the body or casing is found, is one of the main uses of insects in the forensic field. Using information on the biology, ecology and geographical distribution of insects, as well as the behavior of the entire fauna present in a body, is possible to estimate the time of death. Several factors such as temperature, humidity, presence of toxic substances in the tissues of a carcass, may interfere with the life cycle of an insect, directly affecting the estimate of PMI when it is based on biological parameters of the insect. Therefore, multiple factors should be considered so that the forensic analysis is more accurate. With the increase in the number of animal's deaths of economic importance due to drug intoxication, becomes necessary a research on entomotoxicology, an area with lack of specific studies. Thus, the present study aimed to identify the insect fauna associated with carcasses of goats (Capra aegagrus hircus L.) killed after treatment with ivermectin and exposed in the natural environment. Still, investigate possible differences in attractiveness, the immature development that used this substrate for feeding and if the temperature and the colonization pattern of larval mass differ between carcasses of animals killed after ivermectin inoculation. This last parameter was evaluated by thermographic shots performed at intervals of 12 hours. Besides the importance of abiotic factors such as luminosity, temperature, humidity and rainfall, the action of ivermectin on carcasses couse interferense in the composition of the colonizing fauna, the total time of colonization and the time of the decomposition stages, as well as the physical patterns and behavior of larval masses compared to the control group. Although it has been shown that thermography can be used as a new tool in forensic studies, helping to evaluate the parameters of larval mass
Mestrado
Parasitologia
Mestre em Parasitologia

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Paiva, Ana Rita Gomes de. "Farmacogenética em toxicologia forense." Master's thesis, [s.n.], 2014. http://hdl.handle.net/10284/4426.

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Projeto de Pós-Graduação/Dissertação apresentado à Universidade Fernando Pessoa como parte dos requisitos para obtenção do grau de Mestre em Ciências Farmacêuticas
A farmacogenética é a ciência que estuda a influência da componente genética nas respostas a tratamentos farmacológicos. Estas podem variar entre indivíduos devido a vários fatores, sendo um deles a ocorrência de polimorfismos em genes que codifiquem proteínas envolvidas no metabolismo, transporte do fármaco ou que sejam o alvo da ação farmacológica. Os estudos farmacogenéticos têm desempenhado um importante papel na área da toxicologia forense uma vez que acrescentam informações que podem auxiliar na identificação da causa e circunstância da morte, especialmente nos casos em que as concentrações de fármacos encontradas nas análises toxicológicas post mortem são difíceis de interpretar. Estas informações adicionais servem essencialmente para determinar se a morte foi intencional ou acidental, tendo sido publicados vários casos que o demonstram. No entanto, estes estudos apresentam ainda bastantes limitações e são necessárias mais evidências científicas para que sejam implementados na rotina médico-legal e possam ser usados como evidência em tribunal. Apesar deste facto, é amplamente reconhecido que os polimorfismos genéticos podem desempenhar um relevante papel nas mortes e isto alerta para a necessidade da realização de estudos farmacogenéticos aquando da prescrição médica de forma a evitar que tal aconteça. Pharmacogenetics is the science that studies the influence of genetic component in responses to pharmacological treatments. These can vary between individuals due to various factors, one being the occurrence of polymorphisms in genes encoding proteins involved in metabolism, transport of the drug or are the target of pharmacological action. The pharmacogenetics studies have played an important role in the field of forensic toxicology since it adds information that can help to conclude about the cause and manner of death in cases where drugs are found in certain concentrations and thus toxicological results are not clear. This additional information should primarily serve to distinguish intentional and accidental causes and there are several published cases that show that. However, these studies still have many limitations and are needed more scientific evidence before can be implemented in forensic routine and can be used as evidence in court. Despite this fact, there is evidence that genetic polymorphisms may play a role in the deaths and this points to the need of conducting pharmacogenetics studies on prescription to avoid that.

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Spinelli, Eliani. "Identificação de usuários de Cannabis por cromatografia em camada delgada de alta eficiência." Universidade de São Paulo, 1994. http://www.teses.usp.br/teses/disponiveis/9/9137/tde-12122014-171458/.

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A análise de fluidos biológicos para detecção de usuários de Cannabis não é rotina em nossos serviços de toxicologia forense pela falta de um método aplicável às condições de trabalho desses laboratórios. Neste trabalho foi estudado um método que utiliza a cromatografia de camada delgada de alta eficiência (CCDAE) como técnica de identificação. Cinco mililitros de urina são submetidos à hidrólise alcalina e à extração Iíquido/líquido, com posterior aplicação do resíduo obtido na cromatoplaca. O limite de detecção em estudo realizado com adicionados foi de 5ng/ml. Urina de usuários de Cannabis quando submetidas a esta metodologia apresentaram resultado semelhante ao do padrão de THCCOOH, principal produto de biotransformação do THC. As amostras utilizadas como branco de referência não apresentaram mancha semelhante. Na análise das amostras de usuários por imunoensaio de fluorescência polarizada (\"cutoff\' 50ng/ml) obteve-se resultado negativo para usuários moderados e ocasionais. Com auxilio de curva-padrão observou-se que a concentração provável de canabinóides nessas amostras estaria entre 20-50ng/ml. No estudo comparativo dos resultados obtidos nas duas técnicas, foi verificada uma correspondência de 100% para as amostras de usuários com padrão de uso intenso. Nos usuários moderados e ocasionais não foi observada boa correspondência entre os resultados.
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Valente, Nuno Ilídio Pereira. "Análise de pesticidas organofosforados em toxicologia forense." Master's thesis, Universidade de Aveiro, 2012. http://hdl.handle.net/10773/10150.

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Mestrado em Química - Química Analítica e Qualidade
Os pesticidas são substâncias destinadas a prevenir, destruir ou controlar pragas. No entanto, estes produtos são também responsáveis por intoxicações em seres humanos. Em Portugal, mais de metade das intoxicações voluntárias com pesticidas envolvem inseticidas organofosforados (IOFs). Neste trabalho, pretendeu-se desenvolver e validar um conjunto de metodologias para a determinação analítica de dez IOFs, nomeadamente, clorfenvinfos, clorpirifos, diazinão, dimetoato, fentião, fosalona, malatião, paratião, pirimifos-metilo e quinalfos, em amostras de sangue total e de conteúdo gástrico, tendo em vista a introdução das mesmas na rotina pericial do Serviço de Toxicologia Forense da Delegação do Norte do Instituto Nacional de Medicina Legal e Ciências Forenses, I.P. (STF-N). Foram testados métodos de extração de IOFs com Extração em Fase Sólida (SPE) em amostras de sangue com colunas Oasis® HLB e Sep-Pak® C18 e com separação e deteção por GC-ECD e GC-MS. O método de extração com colunas Sep-Pak® C18 foi selecionado, uma vez que no final do processo de extração e análise foram gerados sinais cinco vezes superiores aos obtidos após extração com as outras colunas de SPE, e mostrou ser seletivo para isolamento dos analitos e do padrão interno (etião) em amostras de sangue postmortem. Foram preparadas curvas de calibração entre 50 e 5000 ng/mL, utilizando modelos de regressão linear ponderada. Devido à sensibilidade mais baixa do detetor, não foi possível definir uma gama de trabalho para o fentião por GC-ECD, enquanto para o pirimifos-metilo esta foi estabelecida entre 500 e 5000 ng/mL. O limite de quantificação foi 50 ng/mL para todos os analitos, à exceção do pirimifos-metilo por GC-ECD (500 ng/mL). A eficiência de extração média situou-se entre os 72 e os 102%. Após testes com Extração Líquido-Líquido (LLE) e/ou SPE, o procedimento adotado para rastreio/confirmação qualitativa de IOFs em amostras de conteúdo gástrico, consistiu num passo de LLE com éter dietílico, evaporação do solvente e retoma do extrato em acetonitrilo, seguido de SPE com colunas Sep-Pak® C18 e da análise por GC-MS ou por GC-ECD. Obtiveram-se eficiências de extração médias entre 40 e 50% e limites de deteção de 10 μg/mL para todos os IOFs, exceto para o fentião por GC-ECD. Os métodos desenvolvidos foram considerados robustos e adequados ao propósito, tendo sido já adotados na rotina do laboratório do STF-N.
Pesticides are substances intended to prevent, destroy and control plagues. However, these products are also responsible for intoxications in humans. In Portugal, more than half of pesticide intoxications involve organophosphorus insecticides (OPs). In this thesis we intended to develop and validate methodologies for the determination of ten OPs, namely, chlorfenvinphos, chlorpyrifos, diazinon, dimethoate, fenthion, phosalone, malathion, parathion, pyrimiphos-methyl and quinalphos, in whole blood and gastric content samples, aimed at being included in routine procedures of Forensic Toxicology Laboratory of North Delegation of National Institute of Legal Medicine and Forensic Sciences (FTL-N). In blood, were tested three procedures of Solid Phase Extraction (SPE) for OPs with Oasis® HLB and Sep-Pak® C18 cartridges, followed by GC-ECD and GC-MS analysis. The Sep-Pak® C18 cartridges extraction procedure was selected because the samples prepared using that SPE cartridges generated signals 5 times higher than those obtained with the two different Oasis® HLB cartridges. The method was shown to be selective for the isolation of selected OPs as well as the internal standard (ethion) in postmortem blood samples. Calibration curves Were prepared between 50 and 5000 ng/mL using weighted linear regression models. Due to the lower sensitivity of the detector it was not possible to establish a working range for fenthion by GC-ECD, whereas for pirimiphos-methyl it was set between 500 and 5000 ng/mL. The limit of quantification was 50 ng/mL for all analytes, except for pirimiphos-methyl by GC-ECD analysis (500 ng/mL). The average extraction efficiency was obtained between 72 and 102%. After tests with Liquid-Liquid Extraction (LLE) and/or SPE, the procedure adopted for detection and qualitative confirmation of OPs in gastric content samples consisted in LLE with diethyl ether, solvent evaporation, recovery of the extract with acetonitrile, and SPE with Sep-Pak® C18 cartridges, followed by GC-ECD and GC-MS analysis. Average extraction efficiencies 40 and 50%, and detection limits of 10 μg/mL were obtained by GC-ECD, except for fenthion. The developed methods were considered robust and fit for the purpose, and were already adopted in routine analysis of FTL-N.

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Almeida, Rafael Menck de. "Redistribuição postmortem de barbitúricos em tecidos biológicos humanos." Universidade de São Paulo, 2012. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-12032013-160134/.

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Os barbitúricos são fármacos com atividade depressora do sistema nervoso central e estão relacionados com elevados números de casos de intoxicações e uso não-médico em vários países. No Brasil, a droga antiepiléptica mais encontrada em casos de intoxicação é o fenobarbital, pois os pacientes relatam que \"essa é uma substância com ação forte no cérebro\". De fato, os barbitúricos estão altamente relacionados com tentativa de suicídio e homicídio. Nesses casos existe a necessidade da quantificação dessas substâncias para correlacionar com a causa mortis. No entanto, as análises toxicológicas postmortem são de difícil execução e interpretação, pois a concentração de agentes tóxicos encontrados é bastante complexa e afetada não só pela condição de deterioração do corpo, mas também por um processo conhecido como redistribuição postmortem. Em geral, concentrações mais elevadas são encontradas no sangue situado nos sítios centrais (como o sangue coletado da cavidade cardíaca) em comparação aos níveis verificados nos vasos periféricos (como a veia femoral). Em outros casos, o tempo entre a morte e o exame postmortem é suficiente para que algumas substâncias que normalmente estariam presentes no sangue não estejam mais disponíveis neste fluido biológico. Há ainda um agravante, pois não existem valores de referências para a maioria das amostras biológicas não-convencionais, dificultando assim a interpretação dos resultados. Os exames toxicológicos devem ser realizados em amostras biológicas e tem como objetivo a avaliação da intoxicação como circunstância qualificadora do delito, como causa de periculosidade ou imputabilidade. O objetivo deste trabalho foi o desenvolvimento e aplicação de métodos de identificação de barbitúricos (butalbital, secobarbital, pentobarbital e fenobarbital) em amostras postmortem (sangue cardíaco, sangue femoral e fígado). Os analitos foram extraídos das amostras utilizando a micro extração em fase líquida (LPME), identificados e quantificados por cromatografia em fase gasosa acoplada à espectrometria de massas (GC-MS). Após o desenvolvimento e validação, os métodos analíticos foram aplicados em amostras postmortem de onze cadáveres necropsiados pelo Serviço de Verificação de Óbito da Cidade de São Paulo (SVO (SVO-USP), com suspeita de envolvimento de barbitúricos. Nove casos apresentaram resultado positivo para fenobarbital. A média da razão sangue femoral/sangue cardíaco foi de 0,91 com o desvio padrão de 0,23. Para a correlação fígado/sangue femoral a média foi de 1,17 com desvio padrão de 1,29. Os barbitúricos foram escolhidos como modelo de estudo devido à grande incidência de casos de intoxicação aguda com estes fármacos no Brasil.
Barbiturates are a class of drugs that act as central nervous system depressant and are associated with high numbers of poisoning cases and non-medical use in several countries. In Brazil, phenobarbital is the most related antiepileptic drug involved in intoxication cases. Patients report that \"this drug is a substance with strong action in the brain.\" In fact, barbiturates are highly related to attempted suicide and homicide cases, in which quantification of these substances to correlate with the possible cause of death is necessary. However, postmortem toxicological analyses are difficult to perform and interpret, because the concentration of toxic agents found is quite complex and affected not only by deterioration condition of the body but also by a process known as postmortem redistribution. In general, higher concentrations are found in the blood located in central sites (e.g. heart cavity) compared with the levels found in peripheral vessels (such as the femoral vein). In other cases, the time between death and postmortem examination is enough for some substances that would normally be present in the blood are no longer available in this biological fluid. Besides, there are few reference values for most non-conventional biological samples, making it difficult to interpret the results. The objective of this work was the development and application of methods for identification of barbiturates (butalbital, secobarbital, pentobarbital and phenobarbital) in postmortem samples (heart blood, femoral blood and liver). The analytes were extracted by using liquid-phase micro extraction (LPME) and quantified by gas chromatography-mass spectrometry (GC-MS). After the development and validation, analytical methods were applied in real cases of eleven corpses autopsied by Death Verification Service of São Paulo City (USP-SVO), with suspected of barbiturates involvement. Nine cases were positive for phenobarbital. The mean ratio of blood femoral / cardiac blood was 0.91 with a standard deviation of 0.23. For the correlation liver / femoral blood the average was 1.17 with a standard deviation of 1.29. Barbiturates were chosen as model for this study because the high incidence of cases of acute poisoning with these drugs in Brazil.

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Costa, José Luiz da. "Eletroforese capilar como ferramenta analítica para toxicologia forense." Universidade de São Paulo, 2008. http://www.teses.usp.br/teses/disponiveis/46/46133/tde-23092008-104730/.

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No primeiro capítulo deste trabalho, são apresentados aspectos gerais sobre toxicologia forense e sobre a eletroforese capilar, onde se buscou mostrar como a técnica analítica pode ser útil para aplicações forenses. O segundo capítulo apresenta o desenvolvimento de metodologia analítica baseada em eletroforese capilar com detecção por arranjo de diodos para determinação de drogas de abuso ou seus produtos de biotransformação em humor vítreo. Foram estudados parâmetros como a composição do eletrólito de corrida (com especial atenção ao fenômeno de eletrodispersão), pré-concentração online (stacking) e modo de extração dos analitos. Foi obtida completa separação eletroforética de 12 analitos investigados em menos de 10 minutos de corrida. Os parâmetros de confiança analítica do método mostraram este é perfeitamente aplicável às análises toxicológicas com finalidade forense. O terceiro capítulo apresenta a elaboração de metodologia analítica baseada em eletroforese capilar acoplada a espectrometria de massas para determinação de cocaína e cinco produtos de biotransformação em urina, com procedimento de preparo da amostra biológica simplificado. O procedimento desenvolvido apresentou sensibilidade adequada para verificação de intoxicações agudas por cocaína, e a espectrometria de massas acrescentou grande seletividade à análise, principalmente quando a detecção foi realizada pela seleção do íon-pai e fragmentos gerados a 34% de energia de colisão. O terceiro capítulo apresenta o desenvolvimento de método simples e rápido para determinação de MDMA em comprimidos de Ecstasy usando eletroforese capilar de zona. Na corrida eletroforética desenvolvida, é possível determinar a concentração de MDMA em menos de dois minutos (usando procaína com padrão interno). O método desenvolvido foi comparado ao utilizado rotineiramente no Núcleo de Análise Instrumental do Instituto de Criminalística de São Paulo, baseado em cromatografia líquida de alta eficiência com detecção por fluorescência. O método eletroforético desenvolvido foi cinco vezes mais rápido do que o método de referência, permitindo maior produtividade sem que houvesse perda da qualidade do resultado. Por fim, o capítulo 4 apresenta as considerações finais deste trabalho, onde se pode concluir que a eletroforese capilar, ainda que pouco utilizada em laboratórios forenses brasileiros, pode ser ferramenta de grande utilidade nas análises toxicológicas destinadas a esta finalidade.
In the first chapter of this thesis, general aspects on forensic toxicology and capillary electrophoresis are presented, aiming to show how the analytical technique can be useful for forensic applications. The second chapter presents the development of analytical methodology based on capillary electrophoresis with diode array detection for determining drugs of abuse and/or their biotransformation products in vitreous humor. Parameters such as the composition of background electrolyte (with special attention to the phenomenon of electrodispersion), online pre-concentration (stacking) and sample preparation procedures were objects of study. The complete electrophoretic separation of 12 investigated analytes was obtained within 10 minutes of run. The validation parameters of the method have shown that this is perfectly applicable to toxicological analyses with forensic purposes. The third chapter presents the elaboration of analytical methodology based on capillary electrophoresis coupled to mass spectrometry for determining cocaine and five biotransformation products in urine, with simple sample preparation. The process developed presented adequate sensitivity for the verification of acute intoxications by cocaine, and mass spectrometry contributed with great selectiveness to the analysis, mainly when the detection was conducted by the selection of the molecular-ion and fragments generated at 34% of collision energy. The fourth chapter presents the development of a simple and quick method for determining MDMA in tablets of Ecstasy using capillary zone electrophoresis. In the running condition, it is possible to determine the concentration of MDMA in less than two minutes (using procaine with internal standard). The method developed was compared with the one routinely used at Núcleo de Análise Instrumental do Instituto de Criminalística de São Paulo, based on high performance liquid chromatography with fluorescence detection. The electrophoretic method developed was five times faster than the reference one, allowing higher productivity without loss of quality in the result. Finally, chapter five presents the final considerations of this thesis, where it is possible to conclude that capillary electrophoresis, even being little utilized in Brazilian forensic laboratories, can be a tool of great utility in toxicological analyses destined to this purpose.

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Tremori, Tália Missen [UNESP]. "Cães e gatos: expressão das lesões em intoxicações criminais." Universidade Estadual Paulista (UNESP), 2015. http://hdl.handle.net/11449/131926.

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Os casos de intoxicações não intencionais ou intencionais são comuns na história da Medicina Veterinária principalmente em animais de companhia como cães e gatos. A Medicina Veterinária Legal utiliza amplo conhecimento para fundamentar laudos técnicos que tem como função auxiliar processos judiciais. De acordo com o artigo 32 da Lei de Crimes Ambientais 9.605 de 12 de fevereiro de 1998, intoxicar animais é crime de maus tratos. O reconhecimento adequado dos sinais clínicos, lesões anatomopatológicas características dos casos de intoxicação que levam á óbito associados com os métodos de identificação laboratorial de toxicologia forense, são fundamentais para estabelecer um diagnóstico definitivo do agente tóxico. No presente trabalho objetivou-se ampliar os estudos na área de Medicina Veterinária Legal e identificar lesões anatomopatológicas decorrentes de intoxicação em cães e gatos. No período de 2009 a 2014 foram selecionados do arquivo da Faculdade de Medicina Veterinária e Zootecnia, UNESP - Universidade Estadual Paulista, Campus de Botucatu, Departamento de Clínica Veterinária, Serviço de Patologia Veterinária, 42 casos, sendo 31 (73,8%) cães e 11 (26,2%) gatos. Destes casos 21 (50%) apresentaram Boletim de Ocorrência e 22 (52,4%) realizaram exame toxicológico. A maior prevalência foi de intoxicações por carbamato. O exame necroscópico revelou que a as principais causa mortis foram insuficiência cardiorrespiratória e choque hipovolêmico. No exame histopatológico de fígado, rim e encéfalo as principais lesões observadas foram congestão, degeneração e hemorragia. Os órgãos apresentaram sinais de autólise e putrefação. As técnicas diagnósticas utilizadas são complementares e auxiliam o Médico Veterinário a elaborar laudos técnicos para processos judiciais nos casos de intoxicações criminais
The cases of poisoning no intentional or intentional are common in the history of the Veterinary Medicine mainly in animals of company as dogs and cats. The Legal Veterinary Medicine use these tools in the base of technical decisions to aid processes, involving crimes with animals. According to the Law of Environmental Crimes 9.605 of February 12 of 1998, poisoning in animals is considered crime of mistreatments. The appropriate recognition of the clinical signs, lesions anatomical pathological that characterizes the cases of intoxication that take to death associated with the methods of identification laboratorial of forensic toxicology is fundamental to establish a definitive diagnosis of the toxic agent. In the present work was made analysis of lesions relation of toxic agents and context of Veterinary Forensic Medicine in these situations. In period 2009 to 2014 are selected from the archive of Faculdade de Medicina Veterinária e Zootecnia, UNESP - Universidade Estadual Paulista, Campus de Botucatu, Departamento de Clínica Veterinária, Serviço de Patologia Veterinária 42 cases, 31 (73,8%) dogs and 11 (26,2%) cats. These cases 21 (50%) feature Boletim de Ocorrência and 22 (52,4%) are made toxicologycal exam. The highest prevalence ware intoxication for carbamate. The necropsy revealed that main causa mortis were cardiac respiratory insufficiency and hypovolemic shock. In histopathology of liver, kidney and brain the main lesions are congestion, degeneration and bledding. The organs show signs of autolysis and putrefaction. The diagnostic technics used are additional and help veterinarion to make reports for litigation in cases of criminal intoxication

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Tremori, Tália Missen. "Cães e gatos : expressão das lesões em intoxicações criminais /." Botucatu, 2015. http://hdl.handle.net/11449/131926.

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Orientador: Noeme Souza Rocha
Banca: Elan Cardozo Paes de Almeida
Banca: Alexandre Hataka
Resumo: Os casos de intoxicações não intencionais ou intencionais são comuns na história da Medicina Veterinária principalmente em animais de companhia como cães e gatos. A Medicina Veterinária Legal utiliza amplo conhecimento para fundamentar laudos técnicos que tem como função auxiliar processos judiciais. De acordo com o artigo 32 da Lei de Crimes Ambientais 9.605 de 12 de fevereiro de 1998, intoxicar animais é crime de maus tratos. O reconhecimento adequado dos sinais clínicos, lesões anatomopatológicas características dos casos de intoxicação que levam á óbito associados com os métodos de identificação laboratorial de toxicologia forense, são fundamentais para estabelecer um diagnóstico definitivo do agente tóxico. No presente trabalho objetivou-se ampliar os estudos na área de Medicina Veterinária Legal e identificar lesões anatomopatológicas decorrentes de intoxicação em cães e gatos. No período de 2009 a 2014 foram selecionados do arquivo da Faculdade de Medicina Veterinária e Zootecnia, UNESP - Universidade Estadual Paulista, Campus de Botucatu, Departamento de Clínica Veterinária, Serviço de Patologia Veterinária, 42 casos, sendo 31 (73,8%) cães e 11 (26,2%) gatos. Destes casos 21 (50%) apresentaram Boletim de Ocorrência e 22 (52,4%) realizaram exame toxicológico. A maior prevalência foi de intoxicações por carbamato. O exame necroscópico revelou que a as principais causa mortis foram insuficiência cardiorrespiratória e choque hipovolêmico. No exame histopatológico de fígado, rim e encéfalo as principais lesões observadas foram congestão, degeneração e hemorragia. Os órgãos apresentaram sinais de autólise e putrefação. As técnicas diagnósticas utilizadas são complementares e auxiliam o Médico Veterinário a elaborar laudos técnicos para processos judiciais nos casos de intoxicações criminais
Abstract: The cases of poisoning no intentional or intentional are common in the history of the Veterinary Medicine mainly in animals of company as dogs and cats. The Legal Veterinary Medicine use these tools in the base of technical decisions to aid processes, involving crimes with animals. According to the Law of Environmental Crimes 9.605 of February 12 of 1998, poisoning in animals is considered crime of mistreatments. The appropriate recognition of the clinical signs, lesions anatomical pathological that characterizes the cases of intoxication that take to death associated with the methods of identification laboratorial of forensic toxicology is fundamental to establish a definitive diagnosis of the toxic agent. In the present work was made analysis of lesions relation of toxic agents and context of Veterinary Forensic Medicine in these situations. In period 2009 to 2014 are selected from the archive of Faculdade de Medicina Veterinária e Zootecnia, UNESP - Universidade Estadual Paulista, Campus de Botucatu, Departamento de Clínica Veterinária, Serviço de Patologia Veterinária 42 cases, 31 (73,8%) dogs and 11 (26,2%) cats. These cases 21 (50%) feature Boletim de Ocorrência and 22 (52,4%) are made toxicologycal exam. The highest prevalence ware intoxication for carbamate. The necropsy revealed that main causa mortis were cardiac respiratory insufficiency and hypovolemic shock. In histopathology of liver, kidney and brain the main lesions are congestion, degeneration and bledding. The organs show signs of autolysis and putrefaction. The diagnostic technics used are additional and help veterinarion to make reports for litigation in cases of criminal intoxication
Mestre

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Castro, André Alexandre Lobo Lopes de. "Quantificação de Club Drugs em amostras biológicas em toxicologia forense." Master's thesis, Universidade de Aveiro, 2008. http://hdl.handle.net/10773/3007.

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Mestrado em Métodos Biomoleculares Avançados
As ciências forenses, incluindo a toxicologia forense, apresentam, na actualidade, uma importância acrescida e uma exposição mediática nunca antes atingidas. Os seus resultados são cada vez mais valorizados pelas autoridades judiciais e a sua abrangência é cada vez mais vasta. Tendo como objectivo a aplicação de conhecimentos e métodos científicos na resolução de questões judiciais, a credibilidade e validação das metodologias utilizadas é fulcral para a aceitação de um resultado que terá sempre consequências judiciais. O consumo de substâncias psicoactivas usadas para intensificar fenómenos individuais e colectivos de socialização, associadas a um tipo de sub-cultura organizado ou não em “Clubes de Dança” (dance clubs), denominada Rave Subculture, levanta questões prementes de saúde pública e de envolvimento das autoridades judiciais, quer na prevenção do tráfico, quer na minimização e controlo do seu consumo. As consequências sanitárias e judiciais trazem também as ciências forenses neste plano, justificando a implementação de métodos de detecção e quantificação deste grupo de compostos, quer para avaliação de estado de influenciado, quer para avaliação e determinação de possíveis causas de morte associadas ao seu consumo. Neste trabalho, foi desenvolvido um método de determinação analítica de GHB, GBL, cetamina, propoxifeno, PCP, metadona, flunitrazepam, 7- aminoflunitrazepam e buprenorfina em líquidos biológicos (urina e sangue total) por GC-MS em modo SIM, precedido de extracção por SPE com colunas OASIS® MCX. Os resultados obtidos permitaram a validação da metodologia desenvolvida, a partir de níveis terapêuticos, para a cetamina, propoxifeno, PCP, metadona, flunitrazepam, 7-aminoflunitrazepam e buprenorfina em amostras de urina e sangue total. O método apenas não se mostrou eficaz a concentrações terapêuticas para o flunitrazepam em amostras de urina, com uma taxa de recuperação de 41%. Os restantes compostos apresentaram taxas de recuperação superiores a 68%. Finalmente, o método de extracção não se mostrou eficaz para o GHB e a GBL. Com este método o Serviço de Toxicologia Forense adoptou um procedimento generalista para a detecção deste grupo de substâncias, resultando numa maior rentabilização de recursos físicos e humanos e consequente redução de custos. ABSTRACT: Presently, forensic sciences have been under public authorities’ scrutiny and critical look, due to the increasing attention of the media and public opinion, always applying its aim, the use of scientific knowledge to help solving forensic cases. However, to use forensic toxicology results to solve legal cases, it is crucial to have all the analytical methodologies appropriately validated. The use of psychoactive substances in order to improve social relations and increase body energy in Rave Culture has raised many legal and health public concerns, both for illicit trade and consumption. Forensic toxicology plays an important role in this area, mainly linked to the detection and quantitation of these substances, both in vivo as in post-mortem samples. In this work, we developed a methodology for the extraction and analysis of GHB, GBL, ketamine, propoxyphene, PCP, methadone, flunitrazepam, 7- aminoflunitrazepam and buprenorphine from urine and whole blood samples by SPE (using OASIS® MCX SPE columns) and GC-MS in SIM mode. The results obtained allowed to validate the analytical method for ketamine, propoxyphene, PCP, methadone, flunitrazepam, 7-aminoflunitrazepam and buprenorphine, both for urine and whole blood samples, starting in therapeutic values (except for Flunitrazepam in urine samples, with an extraction efficiency of 41%); all the others compounds shown extraction efficiencies above 68%. Finally the extractive procedure wasn’t efficient both for GHB and GBL. This method constitutes a systematic procedure for club drugs detection able to be routinely applied with evident advantages in terms of a more rational and economic use of equipments and human resources.

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Soares, de Araújo Filho Vanduir. "Aplicação da espectroscopia de ressonância magnética nuclear (RMN) à toxicologia forense." Universidade Federal de Pernambuco, 2006. https://repositorio.ufpe.br/handle/123456789/2034.

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A Ressonância Magnética Nuclear (RMN) e a Cromatografia em fase gasosa acoplada à espectrometria de massas (GC/MS) fornecem informações sobre a estrutura química de substâncias, bem como, sobre a constituição qualitativa e quantitativa de amostras sem a necessidade de padrões de análise ou pré-tratamento de amostras. Uma jovem estudante de 19 anos morreu de forma súbita após inalar um aerossol cujo componente principal, o 1-1-dicloro-1-fluoretano (HCFC-141b), foi identificado por meio de RMN e GC/MS. Nas vísceras e no sangue da vítima não foram detectados venenos, álcool ou outras drogas. Os resultados dos exames necroscópico, toxicológico e microscópico não excluem a hipótese de morte por inalação do HCFC-141b e estabelecem dois mecanismos de morte como viáveis: asfixia e arritmia cardíaca. As análises realizadas e os dados do inquérito policial suportam probabilisticamente a hipótese de morte por arritmia cardíaca fatal que pode ter ocorrido de forma associada com asfixia. Algumas técnicas de RMN como ¹H, ¹³C, Distortionless Enhancement by Polarization Transfer (DEPT), Cross-Polarization and Magic Angle Spinning (CP/MAS) and Dipolar Dephasing (DD) foram usadas para caracterizar amostras de cocaína. Os deslocamentos químicos dos espectros obtidos foram atribuídos por meio de Heteronuclear Correlation (HETCOR) e Heteronuclear Multiple Bond Correlation (HMBC). As amostras foram primariamente caracterizadas por espectrometria de massas cujos espectros foram comparados com dados obtidos na literatura. Os resultados obtidos indicam que ¹H, ¹³C e DEPT são técnicas bastante eficientes para caracterização de amostras ilícitas de cocaína no estado líquido e que por meio de CP/MAS e CP/MAS/DD RMN é possível distinguir o crack do cloridrato de cocaína de uma maneira não destrutiva. Portanto, a RMN é uma excelente ferramenta para caracterização de amostras ilícitas de cocaína

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Santos, Júnior Júlio César 1985. "Novas técnicas analíticas aplicadas a drogas de abuso presentes em humor vítreo." [s.n.], 2014. http://repositorio.unicamp.br/jspui/handle/REPOSIP/312948.

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Orientadores: Nelci Fenalti Höehr, Marcos Nogueira Eberlin
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Ciências Médicas
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Resumo: Embora as anfetaminas estejam proibidas no Brasil, elas continuam sendo adquiridas ilegalmente assim como os canabinóides e cocaína, que representam um dos principais problemas de saúde pública a serem enfrentados no nosso país. Um dos grandes desafios desta área é a dificuldade de obtenção de material para exames periciais. O humor vítreo por encontrar-se isolado em um compartimento relativamente protegido de contaminação externa, invasão de microorganismos e traumatismos em geral, bem como por sua simplicidade/estabilidade analítica e esterilidade durante um longo período após a morte constitui-se como uma excelente amostra para a determinação de xenobióticos em corpos politraumatizados, carbonizados ou em decomposição, auxiliando na delegação da causa mortis. O uso da espectrometria de massas e o advento de novas metodologias de ionização são ferramentas essenciais à toxicologia forense, a V-EASI (venture easy ambient sonic-spray), é uma fonte de ionização de fácil aplicação e instalação, que não requer fluxo de eluente e os demais fatores utilizados nas fontes comerciais. Além disso, o uso da espectrometria de massas de ressonância ciclotrônica de íons por transformada de Fourier (FT-ICR-MS) de ultra-alta resolução e exatidão (valores de m/z exatos) leva a exata composição molecular, alcançando erros abaixo de 1 ppm (partes-por-milhão). Perante isso a avaliação da fórmula molecular normalmente é inequívoca. Quando acoplada a ionização por eletrospray (ESI) espécies moleculares suaves são formadas reduzindo a complexidade do espectro e produzindo informação composicional livre de fragmentos em misturas complexas facilitando sua compreensão. Portanto este trabalho visa o desenvolvimento de metodologias analíticas para análise de drogas de abuso presentes em humor vítreo, empregando o uso de técnicas modernas de espectrometria de massas (FT-ICR-MS e V-EASI-MS)
Abstract: Although amphetamines are banned in Brazil, they remain illegally acquired as cannabinoids and cocaine, which account for a public health task to be faced in this country. The major challenge is to obtain material for investigation exams. The vitreous humor constitutes a good alternative for these exams, since it occurs isolated in a protected space, free of external contamination and of microorganisms and traumatisms, and also due to its analytical stability and sterility preserving it for a long period after death. Moreover, the vitreous humor constitutes an excellent sample for the determination of xenobiotics even in polytraumatized bodies, carbonized or in decomposition, involved in the causa mortis. The use of mass spectrometry and the advent of new ionization methods are essential tools for forensic toxicology, the V-EASI (venture easy ambient sonic-spray), is a source of ionization easy to use and install, not requiring nitrogen flow, eluent flow and other factors used in commercial sources. Furthermore, the use of Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) provides ultra high resolution and accuracy in mass analysis and its accurate m/z values lead to the exact molecular composition, reaching errors below 1 ppm (parts-per-million) on normal operational conditions, the assigned molecular formula are normally unequivocal. When electrospray ionization (ESI) is used, soft molecular species are formed reducing spectra complexity and providing fragment-free compositional information about complex mixtures facilitating comprehension. Therefore, this work aims at the development of analytical methodologies for the analysis of drugs of abuse present in the vitreous humor, employing the use of modern techniques of mass spectrometry (FT-ICR-MS and V-EASI-MS
Mestrado
Ciencias Biomedicas
Mestre em Ciências Médicas

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Tarelho, Sónia Maria Lemos Heleno. "Implementação de técnicas analíticas de determinação de benzodiazepinas aplicadas à toxicologia forense." Master's thesis, Universidade de Aveiro, 2003. http://hdl.handle.net/10773/21704.

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Mestrado em Métodos Instrumentais e Controlo de Qualidade Analítica
O termo “forense” possui um duplo significado. No sentido comum, a ciência forense é entendida como uma disciplina científica particular (medicina, toxicologia, biologia ou química) aplicada às necessidades do direito civil ou criminal. Assim, um sinónimo óbvio de medicina forense é medicina legal. Numa abordagem mais ampla, poder-se-á dizer que todas as disciplinas “forenses” estão sujeitas – mais do que qualquer outra actividade científica – ao debate e ao controlo públicos. Os peritos forenses são obrigados a explicar o mais pequeno pormenor dos métodos utilizados, a fundamentar a escolha das técnicas analíticas aplicadas e a fornecer as suas conclusões imparciais, sob o olhar receoso e crítico dos servidores da justiça, bem como do público em geral, incluindo os media. O resultado final do trabalho dos cientistas forenses exerce influência directa sobre o destino de um determinado indivíduo ou grupo de indivíduos. Esta responsabilidade é o estímulo mais importante para os cientistas forenses, que determina os seus modos de pensar e de actuar. Com este trabalho espera-se contribuir para o esclarecimento judicial de casos relacionados com intoxicações causadas pelo consumo de benzodiazepinas, principalmente quando este conduz à ocorrência de acidentes com implicações judiciais e quando é efectuado em simultâneo com outras drogas (como é exemplo o etanol) que poderão potenciar o efeito tóxico das benzodiazepinas, que por si só possuem toxicidade limitada. Nesta tese, é apresentada, numa primeira fase, uma abordagem geral relativa aos fundamentos da toxicologia e da toxicologia forense, em termos de objectivos, campo de acção, implicações da toxicocinética das substâncias nas determinações analíticas, amostragem, procedimentos de extracção e instrumentação geral. Após a compreensão da arquitectura da toxicologia forense, passa-se à explanação destes conceitos gerais com aplicação específica às benzodiazepinas seguindo-se, então, a apresentação de duas técnicas analíticas para a determinação deste grupo de substâncias: a cromatografia gasosa com detecção por captura electrónica e por espectrometria de massa, com isolamento prévio dos analitos por processos de extracção em fase sólida. A implementação das duas técnicas analíticas acima descritas permite um melhor aproveitamento das capacidades técnicas existentes no Serviço de Toxicologia Forense da Delegação do Porto do Instituto Nacional de Medicina Legal fornecendo, ao mesmo tempo, uma maior quantidade de informação relativa a cada processo, cuja importância é fundamental na eliminação de resultados anómalos. No que diz respeito aos processos de extracção, realizaram-se ensaios em amostras de urina com colunas Bond Elut Certify e em amostras de sangue com colunas Bond Elut Certify e Oasis HLB. No primeiro caso obtiveram-se resultados bastante satisfatórios com rendimentos de extracção superiores a 88%. No caso da extracção de amostras de sangue a eficiência das colunas Oasis HLB mostrou-se bastante superior à das Bond Elut Certify com a obtenção de rendimentos de extracção superiores a 81%, sendo este facto evidente relativamente ao lorazepam para o qual o valor de eficiência assume 10% através da extracção com Bond Elut Certify. Relativamente às técnicas cromatográficas estudadas, no que diz respeito à verificação da qualidade dos resultados, ambas as técnicas permitem a obtenção de coeficientes de variação inferiores aos considerados aceitáveis em ensaios cromatográficos (15%). A cromatografia gasosa com detecção por espectrometria de massa possui aplicação limitada no caso da determinação do lorazepam, do clobazam e do flunitrazepam devido ao facto de fornecer limites de quantificação (9.0, 10.4 e 5.1 ppm, respectivamente) superiores aos valores indicados como tóxicos (superiores a 6, 4 e 3 ppm, respectivamente) e no caso do diazepam para o qual não foi possível a determinação de uma gama de trabalho que permitisse a linearidade da curva de calibração. Por sua vez, a técnica analítica por cromatografia gasosa com detecção por captura electrónica mostrou-se bastante robusta, com a verificação da linearidade de todas as curvas de calibração bem como com a obtenção de limites de detecção e de quantificação aceitáveis (inferiores a 2.7 e 8.2 ppm, respectivamente), permitindo a sua aplicação na determinação de todos os compostos benzodiazepínicos estudados até valores terapêuticos.
The term “forensic” has a double meaning. In the most common sense, forensic science is understood as a particular scientific discipline (medicine, toxicology, biology or chemistry) that is applied for the needs of civil or criminal law. Therefore, an obvious synonym of forensic medicine is legal medicine. In a more wide and deeper sense, all “forensic” disciplines are – more than any other scientific activities – under public debate and control. Forensic experts have tho justify the smallest details of the methods used, to substantiate the choice of the applied technique and to afford their unbiased conclusions, all under the critical and often mistrustful look of the servants of Justice, as well as the general public, including the media. The final result of the forensic scientists activity exerts a direct influence on the fate of a given individual. This responsibility is the driving force, which determines the way of thinking and acting in forensic sciences. This work intends to contribute to the resolution of legal cases related to benzodiazepines consumption, mainly in accidents with legal consequences, and when these compounds are consumed with other drugs (such as ethanol), which, enhance their toxic effect, usually limited. In the first part of this thesis, a general approach is presented in terms of toxicology and forensic toxicology fundamentals such as: aims, field of action, toxicokinetics implications in analytica determinations, sampling, extraction procedures and instrumental methods. After the comprehension of forensic toxicological architecture, this information is linked to specific applications to benzodiazepines and two analytical techniques for benzodiazepines analysis are introduced: gas chromatography with electron capture detector and gas chromatography coupled with mass spectrometry, with previous isolation of the compounds by solid phase extraction. The implementation of the above mentioned methodology in the INML-DP Forensic Toxicology Service allows a rational use of the available techniques, producing relevant analytical data. As extraction procedures are concerned, one have prepared urine assays using solid phase Bond Elut Certify extraction columns and blood assays using solid phase Bond Elut Certify and Oasis HLB extraction columns. In the first case satisfactory results with extraction efficiencies above 88% were obtained. In blood samples, Oasis HLB extraction columns have shown bette efficiency than Bond Elut Certify extraction columns, with extraction efficiencies above 81%. This fact was better proved with lorazepam, which indicated an extraction efficiency of 10% by using Bond Elut Certify extraction columns. The results have shown that the variation coefficients in both chromatographic techniques were well below 15%, the maximum acceptable value in chromatography. Due to high quantification levels obtained for lorazepam, clobazam and flunitrazepam (9.0, 10.4 and 5.1 ppm, respectively), above toxic values (6, 4 and 3 ppm, respectively), and the lack of linearity in calibration curve of diazepam, the application of GC/MS technique is limited. GC/ECD exhibited solid and reproducible results in all the studied benzodiazepines, even for therapeutic levels, with comproved linearity in all calibration curves and reasonable detection and quantification limits (2.7 and 8.2 ppm, respectively).

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Eiras, Marina Marques. "Aplicação de técnica metabolômica em análises toxicológicas forenses de amostras de Cannabis sativa L." [s.n.], 2011. http://repositorio.unicamp.br/jspui/handle/REPOSIP/311826.

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Orientador: Rodrigo Ramos Catharino
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Ciências Médicas
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Resumo: A Cannabis sativa L. é a droga de abuso ilícita mais consumida e apreendida ao redor do mundo. A identificação de Cannabis pode ser alcançada através de diversos métodos, como inspeção visual, cromatografia em camada delgada, cromatografia gasosa e cromatografia líquida, acopladas ou não a espectrometria de massas, entre outros. Entretanto, esses métodos apresentam desvantagens significantes como ambiguidade nos resultados, necessidade de derivatização da amostra, análise relativamente demorada e/ou etapa lenta de preparação da amostra. Neste trabalho, foi desenvolvido um método de fingerprinting metabólico através da técnica de ESI-MS para identificação dos principais canabinóides e aditivos em amostras apreendidas de Cannabis sativa L., para utilização nos laboratórios de toxicologia forense. Ao fazer a determinação instantânea dos compostos das amostras ou fingerprinting metabólico por inserção direta ESI(+)-MS, foi possível observar as diferenças entre os canabinóides e conservantes existentes na Cannabis. O resultado é um fingerprinting metabólico que tem um grande potencial para ser utilizado como método de screening rápido e simples sendo simultaneamente empregado para detectar os canabinóides e conservantes e extrair espectros de diferentes amostras apreendidas em diferentes regiões, além de ser capaz de fazer distinção entre as amostras de uma região e as amostras de outra, o que mostra o potencial da técnica para a certificação de origem geográfica mediante o processo de produção, e possibilidade de ser empregada para outros tipos de drogas de abuso
Abstract: Cannabis sativa L. is the most used and seized drug worldwide. The identification of Cannabis products is achieved by several methods, such as visual inspection, thin layer chromatography, gas chromatography and liquid chromatography coupled or not to mass spectrometry, among others. However, these methods present important disadvantages like ambiguity in the results, the need to sample derivatisation, relatively long analysis or sample preparation. Herein, an ESI-MS metabolic fingerprinting method was tested for the identification of major cannabinoids and additives in seized Cannabis samples, to be used in forensic toxicology laboratories. Instantaneous determination of the sample composition via metabolic fingerprinting by direct insertion ESI(+)-MS reveals the differences in cannabinoids and preservatives in Cannabis samples. The result is a metabolic fingerprinting that has great potential to be used as a fast and simple screening method detecting cannabinoids and preservatives, being simultaneously applied to detect cannabinoids and preservatives and extracting spectra from different samples seized in different regions, besides being able to distinguish them from each other, which shows the potential of the technique to geographical origin certification by processing markers and the possibility to be applied to other types of drugs of abuse
Mestrado
Ciencias Biomedicas
Mestre em Ciências Médicas

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Carvalho, Virgínia Martins. "Redistribuição da cocaína e sua influência na neuroquímica post mortem." Universidade de São Paulo, 2011. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-15072011-120720/.

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A interpretação dos achados laboratoriais no estabelecimento da causa mortis consiste na integração dos conhecimentos sobre a toxicocinética e toxicodinâmica do agente, conhecimentos de sua redistribuição post mortem (RPM) e achados necroscópicos que possibilitem o nexo causal entre o toxicante e o efeito letal. Neste sentido, é importante considerar que somente as concentrações de cocaína (COC) e seus metabólitos podem não ser determinantes na interpretação da causa de morte, podendo ser útil o cotejamento com outros parâmetros, como os níveis de neurotrasmissores que representem o mecanismo de ação do fármaco. Assim, este trabalho teve por objetivo investigar a RPM da COC e seu metabólito benzoilecgonina (BE) em três segmentos do tecido encefálico (TE), no humor vítreo (HV) e sangue (SG), bem como determinar as concentrações de catecolaminas e indolaminas no encéfalo para avaliar a aplicação da neuroquímica post mortem (NPM) na toxicologia forense. No estudo de RPM foram quantificados os níveis de COC e BE em três segmentos do TE (córtex frontal, núcleos da base e cerebelo), no HV e no SG através de método por cromatografia líquida de alta eficiência (HPLC) acoplada ao detector de arranjo de diodos. Os estudos de neuroquímica foram realizados empregando-se HPLC acoplada ao detector eletroquímico. Os resultados indicaram que as concentrações médias de COC foram maiores no TE, seguido por SG e HV (3,09, 2,92 e 1,71 µg/mL, respectivamente), enquanto para BE foram maiores em SG, seguido por HV e TE (6,12, 1,39 e 0,87 µg/mL, respectivamente). As concentrações de COC se apresentaram distribuídas uniformemente nos três segmentos de TE e apresentaram alta correlação com o HV. Adicionalmente, a média de concentrações de dopamina total foi maior no grupo de indivíduos com amostras positivas para COC, sendo verificado diferença significativa entre este grupo e o de indivíduos com amostras negativas para o fármaco de interesse. Os resultados demostraram que o estudo de RPM e da NPM constituem ferramentas aplicáveis na interpretação da causa e maneira de morte.
In case of intoxication, the interpretation of analytical results to assess the cause and process of death requires knowledge about toxicokinetics, toxicodynamic, postmortem redistribution, and autopsy elements. Cocaine-related deaths occur mainly after prolonged drugs use and the presence of cocaine (COC) in fluids or tissues does not prove that death was due to COC consumption, and the interpretation of postmortem concentrations is even more complicated than attempts at making such correlations in the living. The objectives of this study were to investigate the post mortem redistribution (PMR) of COC and its metabolite benzoylecgonine (BE) in three segments of brain (frontal cortex, base nucleous, and cerebellum), vitreous humor, and blood. In additional, catecholamines and indolamines were quantified in brain in order to evaluate the usefulness of post mortem neurochemistry (PMN) in forensic toxicology. In PMR studies were quantified the COC and BE levels in three brain (BR) segments, in vitreous humor (VH), and blood (BL) by High Performance Liquid Chromatography (HPLC) with diode array detection, and for neurochemistry studies the neurotransmitters were quantified by HPLC with electrochemical detection. A homogenous distribution of COC and BE within frontal cortex, base nucleous, and cerebellum was found. The COC media concentrations were 3.09, 2.92 e 1.71µg/mL in BR, BL and VH, respectively, and the BE media concentrations were 6.12, 1.39 e 0.87 µg/mL in BL, VH, and BR, respectively. The COC concentrations in VH show high correlation with brain. The media total dopamine concentration was significant higher in COC positive group. These findings suggest that the studies of PMR and PMN by neurotransmitters levels may be useful to assess the cause and process of death.

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Alzeer, Samar Adnan. "Forensic toxicology of gamma hydroxybutyrate (GHB) metabolism." Thesis, University of Strathclyde, 2011. http://oleg.lib.strath.ac.uk:80/R/?func=dbin-jump-full&object_id=16779.

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Lanaro, Rafael. "Determinação de paraquat e glifosato em amostras de Cannabis sativa encaminhadas para exame pericial." Universidade de São Paulo, 2008. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-27112008-154831/.

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No presente trabalho, foram desenvolvidos e validados dois métodos com o objetivo de determinar os herbicidas paraquat e glifosato, bem como o AMPA, principal metabólito do glifosato, em amostras de maconha apreendidas pela polícia de Campinas, São Paulo. A detecção e quantificação de herbicidas na maconha são necessárias e importantes para alertar o real risco que a droga pode oferecer aos usuários. Existem várias razões que explicam a presença de herbicidas na maconha em vários países, incluindo o Brasil. A eletroforese capilar foi utilizada para determinação dos herbicidas. Um método de detecção direta foi usado para determinar o paraquat e outro, com detecção indireta, para determinar o glifosato e AMPA. Os métodos desenvolvidos mostraram boa linearidade, precisão, exatidão e recuperação. Os dados da validação atestam que os métodos podem ser utilizados em laboratórios Forense no Brasil. Cento e trinta amostras foram analisadas, sendo que em doze amostras foram detectadas a presença de paraquat em várias concentrações e ainda três amostras forneceram resultados positivos apenas para o glifosato sendo uma delas, detectado a presença concomitante do AMPA. Os valores dos contaminantes encontrados podem representar um risco ao usuário, fazendo-se necessário novos estudos para delineamento sobre os reais efeitos que esses contaminantes podem apresentar aos usuários de Cannabis.
In the present work, two methods were developed and validate, aiming to determinate the herbicides paraquat and glyphosate and his major metabolite AMPA in seizured marijuana samples by the police in Campinas, São Paulo. The determination of herbicides in confiscated samples is necessary and important to alert the real risk of marijuana can offer to the users. There are many reasons that explain the presence of herbicides in marijuana in several countries, including Brazil. Capillary electrophoresis was used to determinate the studied herbicides. A method with direct detection was used to determinate paraquat and indirect detection to determinate glyphosate and AMPA. The developed methods showed good linearity, precision, accuracy, and recovery. Therefore, it can be applied in Forensics labs in Brazil. One hundred and thirty samples were analyzed, and twelve of them result positive for paraquat in several concentrations and three samples showed positive to glyphosate and one of them, detected the presence of AMPA. The values of the contaminants found, can offer a risk to the users, making it necessary new studies to know the real effects that such contaminants can offer to the Cannabis users.

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Gordo, José Miguel de Oliveira. "O cabelo como amostra biológica em toxicologia forense: colheita, análise e áreas de aplicação." Master's thesis, [s.n.], 2013. http://hdl.handle.net/10284/3987.

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Projeto de Pós-Graduação/Dissertação apresentado à Universidade Fernando Pessoa como parte dos requisitos para obtenção do grau de Mestre em Ciências Farmacêuticas
Nos últimos anos, a utilização do cabelo como matriz biológica para análises toxicológicas forenses revelou ser uma amostra alternativa importantíssima e, em muitas situações, complementar às matrizes tradicionalmente empregues como o sangue e a urina. A sua capacidade em fornecer ao toxicologista um historial dos compostos consumidos por determinado indivíduo, num período de meses a anos anteriores ao período de colheita, confere a esta matriz propriedades únicas. Atualmente, as análises toxicológicas ao cabelo são aplicadas em diversas áreas tais como crimes facilitados por drogas, controlo de doping, toxicologia post mortem, determinação da exposição a xenobióticos durante a gestação, programas terapêuticos de substituição para toxicodependentes, entre outros. Neste trabalho é feita uma revisão das caraterísticas anatómicas e fisiológicas do cabelo, procedimentos de colheita, metodologias de análise, vantagens e desvantagens da sua utilização na análise de xenobióticos, comparativamente a outras matrizes, bem como possíveis áreas de aplicação dessas análises. Ainda referente a cada uma das áreas de aplicação pretende-se dar enfâse aos principais xenobióticos encontrados. In recent years, the use of hair as biological matrix for forensic toxicology analysis was found to be an important alternative sample and, in many situations, complementary to traditionally used matrices as blood and urine. Its ability to provide toxicologist with a historical profile of an individual´s exposure to drugs or analytes of interest over a period of months to years prior to the harvest period, confers this matrix unique properties. Currently, hair toxicological analysis are applied in various areas such as drug-facilitated crimes, doping control, postmortem toxicology, in utero exposure to xenobiotics, compliance with drug substitution/maintenance therapy, among others. This work is a revision of the hair anatomical and physiological characteristics, sample collection procedures, the analytical methodologies, the advantages and disadvantages of hair use for the analysis of xenobiotics compared to other matrices, as well as the possible applications of hair testing. Still referring to each of the application areas, it is intended to give emphasis to the main xenobiotics found.

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Lourens, Denise. "The epidemiology, pathology and toxicology of suicide." Master's thesis, University of Cape Town, 1998. http://hdl.handle.net/11427/26780.

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Complete suicides and parasuicides are a major cause of death and disability in South Africa and the rest of the world. The epidemiology, pathology and toxicology of complete suicides were investigated in this study. All the complete suicide cases, which were presented to Salt River Medicolegal Laboratory over a period of one year (1 January 1997 - 31 December 1997), were analysed. The candidate personally conducted 148 of the alleged 180 suicide cases that presented in this time period (82%). The candidate did all the follow up investigations herself. The main findings were: 1. The male to female ratio was 5: 1. (131: 26) 2. Shooting and hanging were the most commonly used methods. 3. The racial distribution of violent deaths showed a high rate of suicides amongst the White population. 4. Suicides accounted for the Joss of young lives, the average age being 37,8 years. The mean age was 34 years. 5. Most victims committed suicide in and around their own homes. 6. The majority did not leave suicide notes. 7. Psychiatric disorders, poor health, arguments with close family members and friends, financial problems and long-standing relationship problems were the most common reasons for the suicides. 8. Suicides by prisoners accounted for 3,8% of the study (6 cases). 9. Two cases of double suicide (group suicide) were identified. 10. Five cases of homicide-suicide were identified in the study material. 11. One case of an attempted suicide by means of a high-speed motor vehicle accident, followed by the successful suicide by other means, was identified.

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Peterson, Kristina L. "Advances in flow extraction techniques : applications in forensic toxicology /." Thesis, Connect to this title online; UW restricted, 1997. http://hdl.handle.net/1773/11552.

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Lapachinske, Silvio Fernandes. "Análises físicas e químicas de comprimidos de ecstasy apreendidos no município de São Paulo." Universidade de São Paulo, 2009. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-17072009-114817/.

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Drug profiling, isto é, a caracterização de amostras de drogas apreendidas no sentido de estabelecer conexões entre apreensões realizadas em diferentes épocas e/ou locais a uma origem comum de produção clandestina, tem sido um objetivo dos órgãos governamentais responsáveis pela prevenção/repressão. Especificamente tratando-se de comprimidos de ecstasy, o conhecimento de suas propriedades físicas e químicas é de relevante importância para discriminar a apreensão de diferentes lotes. Nesse contexto, o presente trabalho propõe uma nova abordagem para estabelecer conexões entre apreensões de comprimidos de ecstasy, por meio da calorimetria exploratória diferencial (DSC), termogravimetria (TG) e difratometria de raios-X (DRX). Também foi realizada a caracterização física de todos os comprimidos (logotipo, coloração, massa, diâmetro e espessura), bem como a identificação/quantificação dos constituintes ativos por cromatografia em fase gasosa acoplada à espectrometria de massas (GC-MS) e o perfil de dissolução in vitro. Além disso, foi desenvolvido um método empregando a extração líquido-líquido para o isolamento da 3,4-metilenodioximetanfetamina (MDMA) dos comprimidos de ecstasy, que posteriormente foi cristalizada para cloridrato de MDMA (MDMA.HCl). Foram analisados dezessete diferentes lotes de comprimidos de ecstasy de diversos logotipos e colorações apreendidos no município de São Paulo, Brasil. Apenas um lote apresentou como única substância ativa a clorofenilpiperazina (CPP). Os outros continham apenas MDMA e o conteúdo de MDMA variou de 29 a 115-mg/comprimido. Os valores de massa dos comprimidos variaram de 143 a 341-mg, a espessura de 3,2 a 5,8-mm e o diâmetro de 7,0 a 9,5-mm. A comparação das curvas obtidas, tanto por calorimetria exploratória diferencial (DSC) como pelos difratogramas de raios-X (DRX), permitiu discriminar aqueles com perfis semelhantes, importante para identificar a origem de produção. O baixo grau de cristalinidade do MDMA.HCl de alguns comprimidos de ecstasy não impediu a caracterização por DSC e DRX. Esses resultados podem ser úteis para a aplicação no trabalho de inteligência forense.
Drug profiling or the characterization of seized drug samples to link seizures made at different times and/or locations to their common clandestine origin, has long been a goal of law enforcement agencies. Considering the trafficking of ecstasy tablets, the knowledge of chemical and physical properties is of utmost importance to discriminate between different seizures. In this context this study proposed a new approach to establish links among seizures of ecstasy tablets by using differential scanning calorimetry (DSC), thermogravimetry (TG) and X-ray diffraction (XRD). Besides this characterization, physical appearance (logotype, color, weight, diameter and thickness), identification/quantification of active constituents by gas chromatography/ mass spectrometry (GC/MS) and in vitro drug dissolution assays were performed too. A method employing liquid-liquid extraction was also developed for the isolation of 3,4-methylenedioxymethamphetamine (MDMA) from ecstasy tablets and afterwards MDMA was crystallized to MDMA hydrochloride (MDMA.HCl). Seventeen different lots of various logotypes and colors of confiscated ecstasy tablets from seizures in São Paulo city, Brazil, were analyzed. Chlorophenylpiperazine (CPP) was found only as an active ingredient in one batch. The others tablets contained only MDMA and the content of MDMA varied from 29 to 115-mg/tablet. The weight values of tablets varied from 143 to 341-mg, the thickness from 3,2 to 5,8-mm and the diameter from 7,0 to 9,5-mm. DSC/TG curves and X-ray difratograms of the ecstasy tablets allowed distinguishing those with similar profile, for both techniques, which is important to identify the source of production. The low degree of MDMA.HCl crystallinity of some ecstasy tablets didnt prevent DSC and XRD characterization. These results can be useful for forensic intelligence work application.

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Tormey, William Patrick. "The provision of biochemical investigations in forensic toxicology for coroners." Thesis, Ulster University, 2012. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.646399.

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Death certification plays a central role in health service planning therefore identification of specific causes of death is critical. The requirements of biochemical toxicology as set out in the Coroners Acts in Ireland, Northern Ireland and England and Wales will be parsed to facilitate the construction of a modern best practice template for coroners' toxicology. The Royal College of Pathologists (RCPath) provides published standard guidelines for pathologists reporting to coroners. Their adequacy will be critically evaluated to facilitate reform with the intention of maximising the accuracy of death certification. The roles of psychological factors, tobacco smoking, non steroidal anti-inflammatory drugs, and cannabis in cardiac death will be detailed. The potential for adverse drug reactions to prescription medication to cause death by misadventure will be explored. The role for the expert witness in the inquisitorial coroners system to improve the accuracy of the causes of death and thus the verdict will be explored. My experience has shown that misinterpretation of presence of cannabis in autopsy blood and urine samples is common and this underlines the need for true expert guidance for the coroner. The current practice in biochemical toxicology of screening blood, urine and vitreous humor will be critically evaluated and the necessity for a wide ranging screen of potential toxins as a contributor to the cause of death examined. The appropriate analytes on the screening menu will be determined by local cultural factors. Gas and liquid chromatography with mass spectrometry are the methods of choice. The interpretation of isopropanol, ethanol and ketones in post-mortem blood will be considered as will t~e role of alcohol in death. The apparent population exposure to poisons as reported by Poisons Information Services will be used to explore the dichotomy between the usually benign outcome of common poisons and the often lethal consequences of poisoning by prescription and illicit drugs. The aim of this research is to use the template of the current legal requirements and routine laboratory procedures to suggest reforms which will improve the analytical protocol and reporting of biochemical toxicology in the coronial system resulting in greater accuracy in delineating the causes of death The narrative of this thesis travels through the areas of the coroners acts especially in the Republic of Ireland and the United Kingdom where forensic biochemistry plays a role in the specification of the causes of deaths. There is a deconstruction of the place of doctors in the coronial system and in the new arrangements following the passage of the Coroners and Justice Act 2009 in England and Wales and the potential for change in the Coroners Bill in the Republic of Ireland which fell with the dissolution of the Dail in20ll. There is an examination of the autopsy guidelines issued by the RCPath and suggestions for change which have been published. There is an analysis of the place of cannabinoids in coroners ' cases and publications setting out the position are included. A series of recommendations are made regarding improvement in practice for the reporting of biochemical toxicology in the coronial system. Two cases where there appears to be potential misinterpretation of the toxicological evidence, which may result in the review of the causes of death, are detailed as relevant clinical examples. Some laboratory pitfalls in relation to alcohol analysis have been demonstrated and the consequences of a protocol free service have been detailed with a prescription for improvement and practical solutions to improve outcomes. The under-estimation of the impact of tobacco toxicity is also addressed as is the potential for error due to lack of appreciation of drug-drug interactions. The role of biochemistry in the post-mortem diagnosis of alcoholic and diabetic ketoacidosis is discussed. Multidisciplinary reviews of biochemical toxicology for the coroners' court are suggested as the best safeguard of accurate interpretation to assist coronial enquiry. Conclusions suggesting standard operating procedures for post-mortem scenarios are detailed where possible.

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24

Mullen, Carrie. "Quality Assurance of forensic investigations in toxicology and traffic safety." Thesis, University of Glasgow, 2014. http://theses.gla.ac.uk/5465/.

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The work described in this thesis deals with three aspects of quality assurance in the field of forensic toxicology: proficiency testing schemes, validation of analytical methods for the piperazine group of abused drugs and validation of the police field impairment test, used at the roadside to test drivers for drug-induced impairment. Proficiency Testing: Long term reviews were performed for two forensic external quality assurance schemes. Rounds 30 (in 2007) to 48 (in 2012) of the UKAS-accredited commercial Quartz Forensic Blood Toxicology Proficiency Testing Scheme (PTS), and a ten year period from 1999 to 2009 of the freely-available United Nations Office on Drugs and Crime (UNODC) International Collaborative Exercises (ICE). Only limited ICE data could be made available as much of the original data had been stored on a database which had become obsolete, hence the data were only available as the original results forms provided to UNODC by the ICE participants. Data was entered to Microsoft Excel® spreadsheets and Microsoft Access® databases from the original forms for the years 1999, 2001 (2 rounds), 2003 (2 rounds) and 2005 (2 rounds), and summary data was extracted from the UNODC round reports for the years 2007, 2008 and 2009. Four methods of scoring quantitative performance were reviewed and the most suitable, a z-score using an assigned ‘true’ value and a percentage of the true value as acceptable deviation, was applied to reanalyse the participants’ results and assess their performance. Methods of scoring proficiency which relied upon participants’ data to determine acceptable variation were found merely to describe the data rather than challenge participants on whether or not they were performing fit-for-purpose analyses. Factors such as participation, analytes tested, participants’ methods of analysis and participants performance were summarised for each scheme before the performance of the two schemes, and that of their participants, were compared. ICE tested more analytes per annum but from a smaller test menu than Quartz. This resulted in more repetitive testing and allowed for some trend analysis and performance monitoring. It was not possible to observe performance trends with Quartz due to the wide variety of analytes tested. The smaller array of potential analytes and more repetitive nature of ICE testing also meant that performance monitoring and detection of bias were easier to perform, and ICE was shown to be more effective as external quality assurance (EQA). Quartz provided a good educational resource as it incorporated the wide range of drugs which a forensic toxicology laboratory could realistically encounter. Following the review, however, it was recommended for QUARTZ that, to provide a safeguard against bias, more repetitive testing was required and this has now been adopted. Piperazines: All piperazine analogues are now illegal in the UK, registered as Class C of the Misuse of Drugs Act (1971) and schedule 2, part III of the Misuse of Drugs Regulations (2001). Piperazines can elicit similar effects to some ATS and methods for their detection should be available in forensic toxicology laboratories. In the present study, methods were developed for the detection of a range of piperazines in blood using LC-MS/MS (p-MeOPP, p-FPP, BZP, o-MeOPP, p-MPP and TFMPP) and GC-MS (p-FPP, BZP, TFMPP, p-MPP, o-MeOPP, m-CPP, p-MeOPP and p-CPP). Quality assurance required both methods to be validated. For all piperazine analytes accuracy was within ±15% (20% at low concentrations) and precision was within 15% (20% at low concentrations). For both methods LLOD of all analytes was 5 ng/ml of blood and upper limit of quantification was 2 µg/ml of blood. For the GC-MS method lower limits of quantification (LLOQs) were in the range 20 to 30 ng/ml of blood. For LC-MS/MS, LLOQs ranged from 50 to 60 ng/ml of blood, although quantification by the LC-MS/MS method was restricted by the lack of availability of appropriate internal standards. There were no apparent significant matrix effects and recovery by both methods was >60 % and, therefore, acceptable. Short term stability of the piperazine analytes was investigated. Piperazines remain sufficiently stable when stored in the fridge for at least one week, and are stable through three freeze-thaw cycles. There was no detectable degradation when blood samples were left on the bench-top or when extracted ‘in-process’ samples were left in the autosampler for up to 72 hours. The LC-MS/MS method could provide a readily applicable screening method. A small aliquot of a basic drug extract could be screened by LC-MS/MS for the presence of piperazines, leaving the majority of the extract for other analyses, for example, piperazines confirmation or amphetamines analysis. The GC-MS method was suitably validated to provide quantification but application to casework samples remains to be evaluated. It is recommended that piperazine testing be performed for all suspected MDMA or ‘club drug’ intoxication cases. The Field Impairment Test: The detection of drugged drivers primarily depends on the current method which is the driver field impairment test (FIT). FIT comprises measurement of pupil diameter and four physical tasks (the Romberg balance test, walk and turn test, one legged stand and finger to nose test) intended to simultaneously test comprehension, short term memory, balance and motor function. Despite FIT having ISO accreditation, it has been recognised that police officers lack confidence with the protocol and do not apply the test as often as is necessary. The main difficulty arises from the requirement to make a subjective judgement of impairment and officers lack confidence in their ability to do so. FIT has never been fully validated. The present study was designed to meet the urgent requirement to develop FIT into an objective measurement, by determining what constitutes “normal” performance in FIT by unimpaired adults of different ages. FIT performance was recorded for 79 individuals, a statistically determined cohort size, confirmed by breath and oral fluid analysis not to be under the influence of impairing substances. Each error made during FIT, as defined by the FIT standard operating procedure, was recorded and collated in a Microsoft Excel® spreadsheet for analysis. It was found that the definition of ‘errors’ was too stringent as many which are required to be recorded are normal physiological or behavioural characteristics, such as body sway, and most subjects would be unable to complete the task without displaying them. A less stringent, evidence-based definition of “error” was developed which allowed statistically more significant analysis to be performed on the FIT results. A statistically significant difference (P=0.00578) was shown to exist between the FIT performance of individuals under the age of forty years and those aged forty and over. Based on the principles of a PTS, robust mean and standard deviation were used to determine what constituted acceptable performance. Those in the younger age group could be considered impaired if the police officer witnessed more than seven errors, or, in the older age group, more than fifteen errors. Using these criteria the frequency of false positives, i.e. unimpaired drivers being assessed as impaired is estimated to be (less than 3%). Also, the ranges of errors observed in both groups was large and overlapped, such that it may be possible for an impaired person to appear unimpaired. This requires further investigation.

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25

Yokchue, Tanasiri. "In vitro studies of drug transformations : application to forensic toxicology." Thesis, University of Glasgow, 2016. http://theses.gla.ac.uk/7490/.

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The forensic toxicologist faces challenges in the detection of drugs and poisons in biological samples due to transformations which occur both during life and after death. For example, changes can result from drug metabolism during life or from the use of formalin solution for post mortem embalming purposes. The former requires the identification of drug metabolites and the latter the identification of chemical reaction products in order to know which substances had been administered. The work described in this thesis was aimed at providing ways of tackling these challenges and was divided into two parts. Part 1 investigated the use of in vitro drug metabolism by human liver microsomes (HLM) to obtain information on drug metabolites and Part 2 investigated the chemical reactions of drugs and a carbamate pesticide with formalin solution and formalin-blood. The initial aim of part I was to develop an in vitro metabolism method using HLM, based on a literature review of previous studies of this type. MDMA was chosen as a model compound to develop the HLM method because its metabolism was known and standards of its metabolites were commercially available. In addition, a sensitive and selective method was developed for the identification and quantitation of hydrophilic phase I drug metabolites using LC/MS/MS with a conventional reverse-phase (C18) column. In order to obtain suitable retention factors for polar drug metabolites on this column, acetyl derivatives were evaluated for converting the metabolites to more lipophilic compounds and an optimal separation system was developed. Acetate derivatives were found to be stable in the HPLC mobile phase and to provide good chromatographic separation of the target analytes. In vitro metabolism of MDMA and, subsequently, of other drugs involved incubation of 4 µg drug substance in pH 7.4 buffer with an NADPH generating system (NGS) at 37oC for 90 min with addition of more NGS after 30 min. The reaction was stopped at 90 min by the addition of acetonitrile before extraction of the metabolites. Acetate derivatives of MDMA metabolites were identified by LC/MS/MS using multiple reaction monitoring (MRM). Three phase I metabolites (both major and minor metabolites) of MDMA were detected in HLM samples. 3,4-dihydroxy-methamphetamine and 4-hydroxy-3-methoxymethamphetamine were found to be major metabolites of MDMA whereas 3,4-methylenedioxyamphetamine was found to be a minor metabolite. Subsequently, ten MDMA positive urines were analysed to compare the metabolite patterns with those produced by HLM. An LC/MS method for MDMA and its metabolites in urine samples was developed and validated. The method demonstrated good linearity, accuracy and precision and insignificant matrix effects, with limits of quantitation of 0.025 µg/ml. Moreover, derivatives of MDMA and its metabolites were quantified in all 10 positive human urine samples. The urine metabolite pattern was found to be similar to that from HLM. The second aim of Part 1 was to use the HLM system to study the metabolism of some new psychoactive substances, whose misuse worldwide has necessitated the development of analytical methods for these drugs in biological specimens. Methylone and butylone were selected as representative cathinones and para-methoxyamphetamine (PMA) was chosen as a representative ring-substituted amphetamine, because of the involvement of these drugs in recent drug-related deaths, because of a relative lack of information on their metabolism, and because reference standards of their metabolites were not commercially available. An LC/MS/MS method for the analysis of methylone, butylone, PMA and their metabolites was developed. Three phase I metabolites of methylone and butylone were detected in HLM samples. Ketone reduction to β-OH metabolites and demethylenation to dihydroxy-metabolites were found to be major phase I metabolic pathways of butylone and methylone whereas N-demethylation to nor-methylone and nor-butylone were found to be minor pathways. Also, demethylation to para-hydroxyamphetamine was found to be a major phase I metabolic pathway of PMA whereas β-hydroxylation to β-OH-PMA was found to be a minor pathway. Formaldehyde is used for embalming, to reduce decomposition and preserve cadavers, especially in tropical countries such as Thailand. Drugs present in the body can be exposed to formaldehyde resulting in decreasing concentrations of the original compounds and production of new substances. The aim of part II of the study was to evaluate the in vitro reactions of formaldehyde with selected drug groups including amphetamines (amphetamine, methamphetamine and MDMA), benzodiazepines (alprazolam and diazepam), opiates (morphine, hydromorphone, codeine and hydrocodone) and with a carbamate insecticide (carbosulfan). The study would identify degradation products to serve as markers for the parent compounds when these were no longer detectable. Drugs standards were spiked in 10% formalin solution and 10% formalin blood. Water and whole blood without formalin were used for controls. Samples were analysed by LC/MS/MS at different times from the start, over periods of up to 30 days. Amphetamine, methamphetamine and MDMA were found to rapidly convert to methamphetamine, DMA and MDDMA respectively, in both formalin solution and formalin blood, confirming the Eschweiler-Clarke reaction between amine-containing compounds and formaldehyde. Alprazolam was found to be unstable whereas diazepam was found to be stable in both formalin solution and water. Both were found to hydrolyse in formalin solution and to give open-ring alprazolam and open-ring diazepam. Other alprazolam conversion products attached to paraformaldehyde were detected in both formalin solution and formalin blood. Morphine and codeine were found to be more stable than hydromorphone and hydrocodone in formalin solution. Conversion products of hydromorphone and hydrocodone attached to paraformaldehyde were tentatively identified in formalin solution. Moreover, hydrocodone and hydromorphone rapidly decreased within 24 h in formalin blood and could not be detected after 7 days. Carbosulfan was found to be unstable in formalin solution and was rapidly hydrolysed within 24 h, whereas in water it was stable up to 48 h. Carbofuran was the major degradation product, plus smaller amounts of other products, 3-ketocarbofuran and 3-hydrocarbofuran. By contrast, carbosulfan slowly hydrolysed in formalin-blood and was still detected after 15 days. It was concluded that HLM provide a useful tool for human drug metabolism studies when ethical considerations preclude their controlled administration to humans. The use of chemical derivatisation for hydrophilic compounds such as polar drug metabolites for analysis by LC/MS/MS with a conventional C18 column is effective and inexpensive, and suitable for routine use in the identification and quantitation of drugs and their metabolites. The detection of parent drugs and their metabolites or conversion and decomposition products is potentially very useful for the interpretation of cases in forensic toxicology, especially when the original compounds cannot be observed.

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26

Leite, Flávia Pine. "Determinação de club dugs em sangue total por cromatografia líquida acoplada a espectrometria de massas com analisador híbrido quadrupolo-tempo de voo (LC-QTOF-MS)." Universidade de São Paulo, 2018. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-11062018-110009/.

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As chamadas club drugs compreendem um vasto grupo de substâncias frequentemente utilizadas em bares, festas e raves, com a finalidade de intensificar o contato social e a estimulação sensorial. Englobam desde substâncias sintéticas comumente conhecidas, como a anfetamina, a metanfetamina, o MDMA, até moléculas de surgimento mais recente, denominadas novas substâncias psicoativas. Isoladas ou associadas a outras drogas, é possível que sejam causa de morte per se, ou que predisponham o usuário a envolver-se em situações potencialmente fatais, sendo necessário que os órgãos de Perícia Criminal (Institutos Médico Legais e Institutos de Criminalística) estejam aptos a detectar e quantificar essas substâncias em amostras biológicas. O presente trabalho teve como objetivo desenvolver um método analítico para identificação e quantificação de club drugs em sangue total, utilizando cromatografia líquida acoplada a espectrometria de massas com analisador híbrido quadrupolotempo de voo (LC-QTOF). Após o desenvolvimento do método, este foi validado utilizando as diretrizes do guia de validação do Scientific Working Group for Forensic Toxicology (SWGTOX), sendo analisados de linearidade, limite de detecção, limite de quantificação, efeito matriz, precisão intradia, precisão interdia, exatidão e integridade de diluição, além de recuperação e eficiência do processo. O método desenvolvido compreendeu a determinação de MDA, MDMA, 2C-B, DOB, cetamina, mCPP, cocaína e cocaetileno. Amostras provenientes de casos reais de morte não natural, oriundas do Instituto Médico Legal Aristoclides Teixeira de Goiânia - GO foram analisadas pelo método desenvolvido. 56 casos foram selecionados, em sua maioria com histórico de morte por projétil de arma de fogo e acidente de transito. Das 56 amostras analisadas, 28,5% (n=16) foram positivas para cocaína e/ou cocaetileno. As demais substâncias pesquisadas não foram encontradas nas amostras.
Club drugs are a large group of substances consumed in pubs, parties and raves, aiming to intensify social contact and sensorial stimulation. The term comprises largely known substances such as amphetamine, methamphetamine, 3,4-methylenodioxymethamphetamine (MDMA), as well as so-called new psychoactive substances, which are synthetic drugs recently developed or recently introduced in drug market. Club drugs can be taken alone, combined with each other or, most frequently, with alcohol or other commonly abused drugs such as cocaine. In any of these situations, club drugs can possibly be the cause of death or potentialize the involvement of the user with crime and potentially fatal behavior. Thus, official organisms in charge of criminal investigation must be capable of identifying and quantifying these substances in biological samples. The present work aimed the development of an analytical method to identify and quantify club drugs in whole blood, using liquid chromatography - mass spectrometry with hybrid analyzer quadrupole - time of flight (LC-QTOF). After analytical development, the method was validated according to do Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines, evaluating linearity, limit of detection, limit of quantification, matrix effect, precision, intermediate precision, bias and dilution integrity, besides recovery and process efficiency. The developed method comprised MDA, MDMA, 2C-B, DOB, ketamine, mCPP, cocaine and cocaethylene determination. Real samples related to non-natural deaths were collected at Institute of the Legal Medicine Aristoclides Teixeira, Goiânia, Goiás, Brazil, and analyzed by the developed method. 56 cases were selected, most of them related to fire gun injury and traffic events, 28,5% (n=16) of them being positive for cocaine and/or cocaethylene. None of the other drugs comprised in the analysis were detected in these samples.

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27

Bévalot, Fabien. "Intérêts et limites de la bile et de l'humeur vitrée comme matrices alternatives en toxicologie médicolégale." Thesis, Lyon 1, 2014. http://www.theses.fr/2014LYO10362/document.

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Ce travail avait pour objectif d'étudier l'intérêt et les limites de l'analyse de deux matrices alternatives que sont la bile et l'humeur vitrée (HV), en toxicologie médicolégale. Pour chacune des deux matrices, une revue de la littérature visait à investiguer les connaissances utiles à leur application en toxicologie médicolégale. Une place importante de ces revues est réservée à l'anatomie et la physiologie de l'HV et du système biliaire ainsi qu'aux mécanismes de distribution des xénobiotiques dans ces matrices. La partie expérimentale décrit trois études: deux menées sur populations autopsiques et une associant expérimentations animales et études de populations autopsiques. Les deux premières ont permis de proposer des outils statistiques d'interprétation des concentrations de méprobamate mesurées dans ces matrices. Ils peuvent être utilisés dans diverses situations à la place ou en complément de l'interprétation des concentrations sanguines: cadavre exsangue, putréfaction avancée du corps, redistribution post mortem des xénobiotiques… La troisième étude concernait six molécules (diazépam, citalopram, cyamémazine, morphine, caféine et méprobamate). Les molécules détectées dans le sang l'étaient systématiquement dans l'HV et la bile aussi bien dans les prélèvements des populations autopsiques que ceux issus des expérimentations animales. Les concentrations vitréennes chez l'animal et chez l'homme étaient systématiquement corrélées aux concentrations sanguines, exceptées celles de cyamémazine et de citalopram chez l'homme. Pour la bile, une corrélation significative était observée pour le méprobamate et la caféine chez l'homme et l'animal. Il ressort de ces résultats, que l'analyse de l'HV et de la bile permettent de disposer d'informations relatives à la nature des molécules absorbées et à leur rôle dans la survenue du décès
The present study sought to assess the interest and limitations of analyzing two alternative matrices, bile and vitreous humor (VH), in forensic toxicology. For each matrix, a literature review established the state of knowledge relating to their forensic application. The review placed special focus on the anatomy and physiology of VH and the biliary system and the mechanisms of xenobiotic distribution within the specific matrix. The experimental sections describe three studies: two performed on autopsy populations, and one associating autopsy populations to an animal model. The first two studies resulted in statistical tools for interpreting meprobamate concentrations in these matrices, which can be used as alternatives or complements to blood concentrations in various situations: exsanguination, advanced putrefaction, postmortem xenobiotic redistribution, etc. The third study focused on 6 molecules: diazepam, citalopram, cyamemazine, morphine, caffeine and meprobamate. Molecules detected in blood were also systematically detected in VH and bile samples from both the autopsy and animal populations. Animal VH and blood levels showed systematic correlation. In autopsy samples, cyamemazine and citalopram showed no such correlation. In bile, significant correlations with blood concentrations were found for meprobamate and caffeine in both the autopsy and animal populations. This study confirmed the interest of postmortem analysis of bile and VH. Results show that analyzing bile and VH sheds light on drugs intake and on their implication in cause of death

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28

Costa, José Luiz da. "Determinação de 3,4-metilenodioximetanfetamina (MDMA - Ecstasy), 3,4-metilenodioxietilanfetamina (MDEA - Eve) e 3,4-metilenodioxianfetamina (MDA) em fluidos biológicos por cromatografia líquida de alta eficiência: aspecto forense." Universidade de São Paulo, 2004. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-11032005-190039/.

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Em todo o mundo é crescente o uso drogas de abuso sintéticas conhecidas com designer drugs. Os principais representantes desta classe são o Ecstasy ou 3,4-metilenodioximetanfetamina (MDMA) e o Eve ou 3,4-metilenodioxietilanfetamina (MDEA), substâncias com efeitos estimulantes e alucinógenos. No Brasil é crescente sua divulgação pela mídia e o uso recreacional tem sido constatado em vários pacientes que buscam tratamento nas clínicas para dependentes. O presente trabalho constitui validação de metodologia analítica para o diagnóstico laboratorial do uso de MDMA, MDEA e seu produto de biotransformação, o 3,4-metilenodioxianfetamina (MDA), em sangue total e urina, por cromatografia líquida de alta eficiência com detecção por fluorescência. Os métodos desenvolvidos mostraram boa linearidade, precisão, exatidão, rendimento e capacidade de detectar os analitos mesmos quando presentes em baixas concentrações, o que permite sua aplicação na verificação da intoxicação aguda quanto no uso recreacional destas drogas de abuso.
There is a worldwide increase in the use of the synthetic drugs of abuse known as designer drugs. The main representatives of this class are Ecstasy or 3,4-methylenodioxymethamphetamine (MDMA) and Eve or 3,4- methylenodioxyethylamphetamine (MDEA), substances with stimulant and hallucinogenic effects. In Brazil media coverage of them is on the increase and their recreational is in evidence by the growing numbers of patients who seek treatment at drug treatment centers. This paper validates the analytical methodology for the laboratory diagnosis of the use of MDMA, MDEA and their product of biotransformation, 3,4-methylenodioxyamphetamine (MDA), in whole blood and urine by high performance liquid chromatography with fluorescence. The developed methods showed good linearity, precision, accuracy, yield and capacity to detect analytes even when present in low concentrations, which enables its application in cases high intoxication as well as in cases of the recreational use of these drugs of abuse.

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29

Nilsson, Gunnel. "Zopiclone degradation in biological samples : Characteristics and consequences in forensic toxicology." Doctoral thesis, Linköpings universitet, Avdelningen för läkemedelsforskning, 2014. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-105821.

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Bio-analytical results are influenced by in vivo factors such as genetics, pharmacological and physiological conditions and in vitro factors such as specimen composition, sample additives and storage conditions. Zopiclone (ZOP) is a short-acting hypnotic drug (Imovane®) used for treatment of insomnia. ZOP is metabolized by three major pathways; oxidation to the active zopiclone N-oxide (ZOPNO), demethylation to the inactive N-desmethylzopiclone (NDZOP) and oxidative decarboxylation to other inactive metabolites. ZOP is increasingly being encountered in forensic cases and is a common finding in samples from drug-impaired drivers, users of illicit recreational drugs, victims of drug facilitated sexual assaults and forensic autopsy cases. ZOP is a notoriously unstable analyte in biological matrices and analytical results depend on pre-analytical factors, such as storage time and temperature. The overall aim of this thesis was to investigate the stability of ZOP and the factors of importance for degradation during storage in biological samples and to identify consequences for interpretation of results in forensic toxicology. In paper I, different stability tests in spiked samples were performed including short-term, longterm, freeze-thaw and processed stability. Analyses of ZOP were performed by gas chromatography with nitrogen phosphorous detection and ZOP concentrations were measured at selected time intervals. The degradation product 2-amino-5-chloropyridine (ACP) was identified using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The stability investigations showed a very poor short-term storage stability of ZOP. Therefore, in paper II, the influence of pre-analytical conditions was further investigated in dosed subjects. Whole blood from volunteers was obtained before and after oral administration of Imovane®. In this study, the influence from physiological factors such as drug interactions, matrix composition and plasma protein levels were minimized. The results showed that ZOP was stable in whole blood for only one day at room temperature, one week in a refrigerator and at least three months frozen in authentic as well as in spiked whole blood. The rapid degradation of ZOP at ambient temperature can cause an underestimation of the true concentration and consequently flaw the interpretation. However, by also analyzing the degradation product ACP the original concentration of ZOP may be estimated. In papers III and IV, two LC-MS-MS methods were validated for the quantitation of ACP, ZOP and NDZOP in blood and ACP, ZOP, NDZOP and ZOPNO in urine. These methods were used in a controlled pharmacokinetic study where whole blood and urine were obtained after oral administration of Imovane®. Samples of blood and urine were aliquoted, analyzed and stored under different conditions and the formation of ACP was monitored. Additionally, at each studied time point the pH of the blood and urine samples was measured using i-STAT® system. The results showed that ACP was formed in equimolar amounts to the degradation of ZOP and its metabolites. In urine samples, the formation of ACP occurred at elevated pH or temperature and mirrored the degradation of ZOP, NDZOP and ZOPNO. The high concentrations of metabolites, which also degraded to ACP, made it impossible to estimate the original ZOP concentration. The results from analysis of blood samples containing ACP were also used to develop mathematical models to estimate the original ZOP concentration. Both models showed strong correlation to the original ZOP concentration (r=0.960 and r=0.955) with p<0.01. This study showed that the equimolar degradation of ZOP and NDZOP to ACP could be used to estimate the original concentration of ZOP in blood samples. Absence of ACP in the blood or urine samples analysed strongly suggests that degradation has not occurred and that the measured concentration of ZOP is reliable. For proper interpretation in forensic cases, it is strongly recommended that ZOP and its metabolites as well as ACP are included in the analysis.

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30

Takaichi, Kenichi. "Nail analysis in forensic toxicology for the detection of drug misuse." Thesis, University of Glasgow, 2004. http://theses.gla.ac.uk/3533/.

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This thesis examines the use of nail as an alternative biological specimen in forensic toxicology. Nail is a difficult analytical matrix from which to extract drugs because of its tough physical composition, based on keratin. The initial part of the project investigated the use of a cryogenic grinding method for fingernail clippings. Grinding at liquid nitrogen temperatures was found to be an effective procedure and the conditions were optimised to a two or three cycle programme of freezing and grinding. Small particle sizes were obtained of approximate size 1µm. It was established that drugs could be extracted directly from nail powder with a range of solvents without the need for alkaline hydrolysis. Methanol was found to be the most effective extraction solvent, which also gave the lowest number of co-extracted interfering compounds. This procedure was subsequently used with nail samples from different types of forensic cases, including cannabis, heroin and steroid abusers. Cryogenic grinding of nail was evaluated as an extraction method for cannabinoids in nail clippings from chronic cannabis smokers. This method was also compared to the alkaline hydrolysis method. Fingernail clippings were collected with prior informed consent from volunteers attending the Edinburgh Drug Addiction Study (EDAS) clinic. The collected nail clippings were decontaminated and divided into two groups: the first group was extracted with methanol after pulverisation in a liquid nitrogen cryogenic mill; the second was extracted with ethyl acetate after hydrolysis in sodium hydroxide. In both groups deuterated cannabinoids were used as internal standards. Both sets of extracts were derivatised with BSTFA before being analysed by gas chromatography – mass spectrometry (GC-MS). Cannabidiol, ?9-tetrahydrocannabinol and 11-hydroxy-?9-tetrahydrocannibinol were quantified in both sets of extracts. 11-nor-?9 –tetrahydrocannabinol-9-carboxylic acid was only identified and quantified in the extracts resulting from the cryogenic grinding method. Cannabinoid concentrations were very low, in the range 0-4 ng/mg. These results strongly support the use of nail as a biological specimen for the detection and quantification of past exposure to cannabis, and secondly, they indicate that grinding with a cryogenic mill is a useful procedure, which yields simultaneous results for the primary psychoactive cannabinoid and its metabolites. Cryogenic grinding was then evaluated for the extraction of opioids in nail in comparison with the conventional alkaline hydrolysis method. Finger and toe nails were collected from donors with informed consent.

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31

Ariffin, Marinah Mohd. "The application of novel extraction and analytical techniques in forensic toxicology." Thesis, University of Glasgow, 2006. http://theses.gla.ac.uk/4144/.

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The aim of this study was to investigate new methods of analysis which might be applied to forensic toxicology problems including those resulting from pesticides, particularly the quaternary ammonium herbicide group, and from drugs, particularly the benzodiazepine group. In the first part of this study, an efficient method for the determination of quaternary ammonium (QA) compounds (pesticides and drugs) in human whole blood was developed. The second part of this study concerned the development of a novel sorbents for solid phase extraction using molecularly imprinted polymers (MIPs). The approach adopted was initially to synthesise a known MIP using diazepam as template then to prepare novel MIPs using other benzodiazepines and analogues of QA compounds as templates. In the first of these stages, an anti-diazepam MIP was synthesized using methacrylate acid (MAA) as the monomer and ethylene glycol dimethacrylate (EGDMA) as the cross-liner and was then ground and prepared for use as an SPE sorbent by packing it into SPE cartridges. These cartridges were used to clean up extracts of diazepam and other benzodiazepine drugs made from hair samples via a molecularly imprinted solid-phase extraction (MISPE) protocol. The MISPE method was also found to be applicable to the analysis of diazepam metabolites and other benzodiazepine drugs in addition to diazepam itself. The application of the extraction method to post-mortem hair samples yielded results that were in good agreement with ELISA data (from blood samples) and data arising from the analysis of the same blood samples using a validated in-house SPE-LC-MS-MS method. The MISPE procedure was also compared with a conventional SPE method for analysis of benzodiazepines in hair samples. The results from MISPE protocol showed better selectivity, specificity and accuracy toward diazepam (template molecule) and other benzodiazepines that display a similar resemblance to diazepam in terms of molecular structure. The MISPE procedure was found to be simpler and to offer cleaner extracts compared to a conventional SPE method.

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Holmgren, Per. "Postmortem toxicology : aspects on interpretation /." Linköping : Univ, 2004. http://www.bibl.liu.se/liupubl/disp/disp2004/med862s.pdf.

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33

Pericolo, Suellen. "Cocaína e cocaetileno em mortes violentas." reponame:Repositório Institucional da UFSC, 2016. https://repositorio.ufsc.br/xmlui/handle/123456789/173270.

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Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro de Ciências Biológicas, Programa de Pós-Graduação em Farmacologia, Florianópolis, 2016.
Made available in DSpace on 2017-02-14T03:07:40Z (GMT). No. of bitstreams: 1 343684.pdf: 3983252 bytes, checksum: 9c21e57851242970d9839907700965a0 (MD5) Previous issue date: 2016
A utilização intencional de substâncias modificadoras do estado de consciência é prática milenar entre as civilizações. O consumo abusivo na sociedade contemporânea cresce vertiginosamente, disseminado por todas as esferas sociais, fomentando um rentável e disputado mercado ilegal. A íntima relação do uso de drogas e mortes violentas é tema amplamente debatido em levantamentos e estudos científicos. O conhecimento do perfil destes óbitos e as substâncias mais recorrentes alicerçam o desenvolvimento técnico-científico para atender às especificidades desta demanda. O Instituto Geral de Perícias de Joinville (IGP/Joinville) conta com software institucional que armazena dados relacionados aos atendimentos e os respectivos laudos das ocorrências, viabilizando levantamentos desta natureza. No âmbito forense a realização de exames toxicológicos é importante ferramenta para auxiliar na determinação da causa morte. Todavia, o estado do cadáver pode ser fator limitante para a coleta de espécimes de referência. O humor vítreo (HV) figura como matriz alternativa de grande aplicabilidade por apresentar boa correlação com os níveis sanguíneos. A microextração em fase sólida (SPME) destaca-se pela alta sensibilidade, fácil execução, viabiliza a análise de pequenos volumes e integração automatizada ao cromatógrafo gasoso com espectrômetro de massas (GC/MS). O presente estudo efetuou levantamento do perfil de óbitos atendidos pelo IGP/Joinville no período de 2013 a 2015, ponderando a natureza jurídica das mortes distribuídas em homicídios, suicídios, acidentes de trânsito e outras formas, o gênero e a idade das vítimas, a coleta de amostras biológicas e as substâncias mais detectadas. Os acidentes de trânsito compreenderam o maior número de óbitos, abrangendo 40,9% dos casos, seguidos por homicídios com 29%, enquanto os suicídios contabilizaram 9,1% e outras formas de morte 21%. Entre as amostras não coletadas as justificativas se alternaram entre óbitos em ambiente hospitalar (54,1%), cadáveres putrefeitos (7,7%), carbonizados (0,6%), politraumatizados (1,3%), ossadas (0,9%) e não justificados (35,4%). Os homicídios abarcaram o maior percentual de toxicológicos detectados (70,5%). Os suicídios apresentaram detecção em 51,6%, acidentes de trânsito em 50% e outras formas de morte em 51,9% dos casos. A cocaína (COC) foi a substância ilícita mais recorrente entre as classificações de morte com exposição concomitante ao álcool. A exposição associada leva a formação do cocaetileno (CE), composto mais tóxico que os precursores. Diante deste cenário, foi validado método para a detecção de COC e CE em HV por SPME e GC/MS. A técnica compreendeu a análise de 0,5 mL de HV, adicionados de 1,0 mL de tampão borato, extração por SPME (fibra DVB/PDMS) sob temperatura (60ºC) e agitação constantes durante 20 min., exposição da fibra no injetor a 250ºC por 5 min e limpeza a 250ºC por 5 min. O método demonstrou precisão sob repetibilidade, apresentando coeficientes de variação (CVs) dos tempos de retenção de 0,4% e 0,3% para COC e CE respectivamente, limite de detecção estipulado em 5 ng/mL com CVs de triplicatas inferiores a 20%, ausência de interferentes na detecção dos analitos de interesse, considerando-se os compostos nicotina, lidocaína e cafeína, e procedimento de limpeza eficaz para a eliminação do efeito carryover. A aplicação do método em amostras post mortem de HV reproduziu os resultados de detecção obtidos em sangue e urina, assim como confirmou a não detecção dos analitos nos casos negativos testados. Os achados demonstraram a viabilidade de emprego do HV na ausência das matrizes de referência e a importância da coleta de matrizes diversificadas visando ampliar a janela de detecção dos analitos de interesse.

Abstract : The intentional use of substances that modify the state of consciousness has been happening for thousands of years among civilizations. The abusive use in the contemporary society has grown wildly, is has been spread by all social spheres, fostering a profitable and disputed illegal market. The close relation between the use of drugs and violent deaths is an issue widely discussed in surveys and scientific researches. The knowledge about the profile of these deaths and the most recurrent substances, anchors the scientific development to meet the needs of these demands. The Instituto Geral de Perícias de Joinville (IGP/Joinville) has institutional software that store data related to the attendance and respective occurrence reports, making surveys of this kind feasible. In the forensic scope, the procedure of toxic exams is a very important tool to determine the cause of death. Nevertheless, the state of the corpse may be a limiting factor when it comes to collecting reference specimen. The vitreous humor (VH) features as alternative matrix of big applicability for showing good correlation with blood levels. The extraction by solid phase microextraction (SPME) stands out for high sensibility, easiness to use, making feasible the analysis of small volumes and automated integration to gas chromatography-mass spectrometry (GC/MS). The presented study has carried out a survey about the profile of deaths assisted by IGP/Joinville between the years 2013 and 2015, considering the legal status of the deaths among homicide, suicides, traffic accidents and others, gender, victims age, collection of biological samples and the most detected substances. Traffic accidents make the highest number of deaths, comprehending 40,9% of occurrences, followed by homicides with 29%, other forms of deaths with 21% and suicides with 9,1%. Among the cases not collected the reasons are deaths in hospitals (54,1%), putrefied corpses (7,7%), burned corpses (0,6%), multiple-injured bodies (1,3%), bones (0,9%) and non justifies (35,4%). The homicides comprised the biggest percentage of positive toxicological (70,5%) followed by others (51,9%), suicides (51,6%) and traffic accidents (50%). The cocaine (COC) was the most detected compound in all deaths classification with concomitantly consumption of alcohol. They lead to formation of cocaethylene (CE), compound that is more toxic than the former ones. In this situation, the method for detection of COC and CE was validated in VH by SPME and GC/MS. The technique includes the addiction of 0,5 mL of VH and 1,0 mL of borax buffer, exposed to SPME (DVB/PDMS fiber) for 20 min at 60ºC and constant agitation. After the fiber was exposed in the inlet (250ºC) for 5 min and then cleaned for 5 min at 250ºC. The method has shown precision on repeatability with coefficient of variation (CVs) of retention time by 0,4% (COC) and 0,3% (CE), limit of detection estimated in 5 ng/mL with CVs of triplicates lower than 20%, absence of interfering compounds in the detection of analytes of interest, considering the compounds nicotine, lidocaine and caffeine, and procedures of effective cleaning in order to eliminate the carryover effect. The application of this method in post mortem samples of VH has shown correlation with the positive results obtained by COC and CE in blood and urine, as well as it has confirmed the non-detection of analytes in tested negatives. The findings have shown the importance of varied matrix collection in order to enlarge the window of detection and the feasibility of the use of VH in the absence of reference matrixes.

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34

Curtis, Byron Dale. "The forensic toxicology of 2,5-dimethoxy-4-n-propylthiophenethylamine (2C-T-7)." Oklahoma City : [s.n.], 2005.

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35

Lemos, Nikolaos P. "Analysis of bile and nail as alternative biological specimens in forensic toxicology." Thesis, University of Glasgow, 1999. http://theses.gla.ac.uk/4116/.

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This thesis examines the use of bile and nail as alternative biological specimens in forensic toxicology. In chapter 1, a brief overview of the mechanisms of substance passage into and out of membranes and fluids and matrices was presented followed by a review of the use of alternative biological specimens for analytical purposes. The experimental part of this thesis begins in chapter 2 where a simple and rapid method for the detection and quantification of dextropropoxyphene in bile and its major metabolite, norpropoxyphene, is presented. Following this, nail is examined as an alternative biological specimen in cases of medico-legal interest. Firstly, two major cannabinoids, 9-tetrahydrocannabinol and 11-nor-9-tetrahydrocannabinol-9-carboxylic acid were identified in the nail (chapter 3) by means of RIA and GC-MS. Cannabinoids were found to be present in all six cases that were analysed for cannabinoids by RIA and their concentration ranged from 0.23 ng/mg to 2.80 ng/mg (average: 1.03 ng/mg). Using GC-MS, 9-tetrahydrocannabinol was detected in 11 out of the 14 nail clipping hydrolysates after basic extraction with concentrations ranging from 0.13 ng/mg to 6.97 ng/mg (average: 1.44 ng/mg). 11-nor-9-tetrahydrocannabinol-9-carboxylic acid was not detected in any of these nail clipping hydrolysates but was detected in two of the three fingernail clipping hydrolysates extracted under acidic pH with concentrations ranging from 9.82 ng/mg to 29.7 ng/mg (average: 19.8 ng/mg). In chapter 4, the detection and quantification of diazepam, the most commonly encountered benzodiazepine, were described. Using ECD-GC, diazepam was detected in hydrolysates of all 6 sets of nail clippings in concentrations ranging from 4.37 to 87.8 ng/mg (average: 25.7 ng/mg). In chapter 5, an analytical protocol for the detection and quantification of morphine in nail clippings of known heroin abusers was presented. Finally, a protocol for the detection and quantification of methadone in nail clippings of patients attending a methadone maintenance program was presented.

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Siqueira, Adriana de. "Avaliação dos efeitos tóxicos dos carbamatos: I. Modelo experimental em ratos Wistar e comparação com a intoxicação exógena intencional em gatos e cães; II. Análise de estabilidade dos compostos e dos seus efeitos nos post mortem imediato e em animais exumados." Universidade de São Paulo, 2015. http://www.teses.usp.br/teses/disponiveis/10/10133/tde-31082015-142508/.

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A intoxicação intencional de animais e de pessoas é uma ameaça à saúde e à segurança públicas em todo o mundo. No Brasil, os pesticidas da classe dos carbamatos aldicarbe e carbofurano são facilmente obtidos, e uma única dose letal daqueles é facilmente misturada a alimentos palatáveis e iscas. Foram analisadas as necropsias de 26 gatos e 10 cães, da rotina do Serviço de Patologia Animal da FMVZ-USP, com variados intervalos post mortem e tipos de conservação de carcaça, intoxicados pelos carbamatos aldicarbe e carbofurano, confirmados pela cromatografia de camada delgada (CCD) e cromatografia líquida de alta performance com detector de arranjo de diodos (CLAE-DAD). Foram colhidas as matrizes biológicas para histopatologia e análise toxicológica. CLAE-DAD foi utilizada para detectar o aldicarbe e seus metabólitos, aldicarbe sulfóxido e aldicarbe sulfona, e carbofurano e seu metabólito 3-hidroxicarbofurano. As análises macroscópica e histopatológica revelaram predominantemente achados congestivos e hemorrágicos, o que pode ser resultante dos efeitos tóxicos dos carbamatos e seus metabólitos. Foram feitos 2 experimentos envolvendo exposição a uma dose única de carbofurano e de aldicarbe via gavagem em ratos Wistar. No primeiro, no qual foram avaliados os efeitos no post mortem imediato, 30 animais forma separados nos seguintes grupos: aldicarbe (n=10), carbofurano (n=10) e grupo controle (n=10). Os animais foram filmados para avaliar as alterações clínicas na intoxicação aguda e, quando foram sedados, foi colhido sangue por punção cardíaca para fazer o hemograma, bioquímica sérica, colinesterase e exame toxicológico e, após a eutanásia, foi feita a necropsia e colhido material para o exame histopatológico. Em todos os animais experimentais foi possível ser feita a detecção e a quantificação do aldicarbe e do carbofurano, além das alterações microscópicas congestivas e hemorrágicas, com alterações em parâmetros hematológicos e bioquímicos. No segundo experimento, foram utilizados 30 animais, e o protocolo experimental foi idêntico ao experimento anterior, exceto que, após o óbito, os animais foram colocados em uma caixa com terra nos seguintes grupos: 1 dia, 3 dias, 5 dias, 7 dias e 10 dias, e em cada dia foram agrupados 2 animais intoxicados e 1 controle, sendo que as necropsias foram feitas nestes intervalos. Foram colhidos cérebro, pulmão, fígado e rim ao exame histopatológico e globo ocular, conteúdo gástrico, fígado e músculo esquelético ao exame toxicológico. Foram observadas as alterações tanatológicas e, em todas as matrizes analisadas, puderam ser quantificados o aldicarbe e/ou seus metabólitos aldicarbe sulfóxido e aldicarbe sulfona, bem como o carbofurano e seu metabólito 3-hidroxicarbofurano. Estes estudos mostram a importância da necropsia e da coleta de matrizes diversas ao exame toxicológico, que são complementares e cruciais na investigação de óbitos decorrentes de intoxicações por praguicidas, tanto no post mortem imediato quanto em exumações
The intentional poisoning of animals and people is a threat to public health and safety worldwide. In Brazil, the carbamate pesticides aldicarb and carbofuran are easily obtained. A single lethal dose of these carbamates is easily mixed with palatable food or baits. Necropsies and histopathological examinations of 26 cats and 10 dogs poisoned by the carbamates aldicarb and carbofuran were performed in the Service of Animal Pathology of FMVZ-USP, and the poisoning was confirmed by thin layer chromatography (TLC) and high performance liquid chromatography with diode-array detector (HPLC-DAD), with variable post mortem interval and conservation of the carcass. Biological matrices were collected for histopathological and toxicological analysis. HPLC-DAD was utilised to detect aldicarb and its metabolites, aldicarb sulphoxide and aldicarb sulphone, and carbofuran and its metabolite 3-hydroxycarbofuran. Gross and histopathological evaluations showed mainly congestive and haemorrhagic findings, which may result from the toxic effects of the carbamates and their metabolites. Two experimental protocols were performed in Wistar rats by exposing them to a single oral gavage dose to the carbamates aldicarb and carbofuran. The first experiment was performed to evaluate the immediate post mortem effects of carbamates, and 30 rats were divided into three groups: aldicarb (n-=10), carbofuran (n=10) and control (n=10). The animals were filmed to evaluate the clinical signs of poisoning, and they were sedated to collect blood by heart puncture, to perform CBC, serum biochemistry, and to measure serum cholinesterase. After euthanasia, tissues were collected for histopathological evaluation. Aldicarb and carbofuran were detected and quantified in the blood of all experimental groups, and the most common histological changes observed were congestion and haemorrhage. In the second experiment, the experimental protocol was identical to the first one, but the animals were buried in a plastic box with garden soil within 5 groups of 3 animals, two exposed to the same pesticide and 1 control, as follows: day 1, day 3, day 5, day 7 and day 10. The exhumations were performed within these days (1, 3, 5, 7 and 10). We collected brain, lung, liver and kidney to examine the thanatological changes, and the eyeballs, gastric content, liver and skeletal muscle to perform the toxicological screening. Thanatological changes could be observed within and between the groups, and, in all the matrices we could detect aldicarb and its metabolites aldicarb sulphoxide and aldicarb sulphone, and carbofuran and its metabolite 3-hydroxycarbofuran. The studies have shown the importance of the necropsy and the collection of diverse matrices to the toxicological screening, because both are complementary and crucial to the investigation of deaths by pesticides poisoning, even in exhumation, since we could evaluate the thanatological changes and correlate them to the action of the pesticides in the tissues

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Carvalho, Virgínia Martins. "Pesquisa dos indicadores de uso do \"crack\" em amostras de urina de indivíduos submetidos a exame médico-legal." Universidade de São Paulo, 2006. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-16052007-202416/.

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Atualmente os dados epidemiológicos sobre a exposição ao crack no Brasil são preocupantes, principalmente entre crianças e adolescentes na capital de São Paulo. É sabido que o crack apresenta um potencial maior que o correspondente a outras formas de uso da cocaína para causar dependência. Apesar de haver numerosos estudos e métodos validados para identificação e quantificação de cocaína em fluidos biológicos, o mesmo não ocorre para a caracterização de seu uso na forma de crack. Todos os métodos descritos para diferenciação de exposição ao crack empregam equipamentos de alto custo e que nem sempre são viáveis para a realidade econômica dos laboratórios públicos brasileiros. Este trabalho objetivou desenvolver e aplicar um método eficiente e viável economicamente para identificação e quantificação dos indicadores de uso do crack em amostras de urina provenientes do Núcleo de Toxicologia Forense do Instituto Médico-Legal de São Paulo. O método mostrou-se linear na faixa de interesse (intervalo dinâmico de 0,2 a 20 µg/mL) para éster metilanidroecgonina. Os limites de detecção e quantificação foram de 0,1 e 0,2 µg/mL respectivamente e os testes de estabilidade mostraram-se satisfatórios (degradação menor que 10% após 30 dias). Foram analisadas trinta e sete amostras de urina sendo que onze foram positivas para o indicador escolhido mostrando a utilidade do método no esclarecimento de ocorrências no âmbito forense, no sentido de indicar se a intoxicação da cocaína se deu por esta forma de exposição (utilização de crack).
At the present time, epidemiologic data on the prevalence of crack in Brazil is alarming, principally as it concerns young children and teenagers in the capital city of São Paulo of São Paulo State. It is known that with crack there is a greater potential for dependency than that corresponding to other forms of cocaine use in causing dependency. Although numerous studies and methods have been validated for the identification and quantification of cocaine in biological fluids, the same is not true for the characterization of its use in the form of crack. All the methods described for differentiating the exposure to crack employ very expensive equipment, which is not always viable to the economic reality of the Brazilian public laboratories. This study had as its objective the development and application of a method that is efficient and economically viable for the identification and quantification of products of crack biomarkers in urine samples from the Forensic Toxicology Lab of the Legal Medicine Institute of São Paulo. The method showed to be linear in the interest range (dynamic range from 0.2 to 20 µg/mL ) for anhydroecgonine methyl ester. The limits of detection and quantification were 0.1 and 0.2 µg/mL respectively, and the stability tests proved to be satisfactory (less than 10% lost after 30 days). Thirty seven urine samples were analyzed such that these 11 were positive for the chosen biomarker, showing the usefulness of the method for clarification purposes in the forensic environment, in the sense of indicating whether the intoxication from cocaine was of this form of exposition (crack use).

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38

Al-Ahmadi, Tareq Mohammed. "A comparison of derivatisation procedures for the detection of multiple analytes in systematic forensic toxicology." Connect to e-thesis, 2007. http://theses.gla.ac.uk/948/.

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Thesis (Ph.D.) - University of Glasgow, 2007.
Ph.D. thesis submitted to the Department of Forensic Medicine and Science, University of Glasgow, 2007. Includes bibliographical references. Print version also available.

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39

Gerostamoulos, Jim 1969. "The toxicological interpretation of heroin-related deaths." Monash University, Dept. of Forensic Medicine, 1997. http://arrow.monash.edu.au/hdl/1959.1/7770.

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40

Torrance, Hazel Jennifer. "An investigation into the potential use of liquid chromatography:mass spectrometry in forensic toxicology." Thesis, University of Glasgow, 2005. http://theses.gla.ac.uk/4122/.

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The aim of this project was to evaluate the use of LC-MS in the forensic toxicology setting. To investigate if its use could solve problems encountered while using other instrumentation including downtime, limits of detection, chromatography and specificity. Benzodiazepines as a class, are known for their undesirable chromatographic behaviour when using GC. Using LC-MS two models were developed for the analysis of these drugs in whole blood. Increasing awareness of drug facilitated sexual assault, has led to an increase in the number of cases to be analysed for drugs such as Rohypnol®. This prompted the development and validation of a sensitive and specific method for its detection in blood using solid phase extraction and liquid chromatography – mass spectrometry. To enhance the qualitative data and cope with degraded samples, the use of LC-MS was used in the analysis of diazepam and its three metabolites. A method was developed and validated and is now used in the routine analysis of blood samples in the laboratory. The LC-MS proved invaluable in the analysis of sildenafil, Viagra®, in a post-mortem blood sample received in the laboratory. A single quadrupole mass spectrometer was used to develop and validate a method to determine if the dose was therapeutic or toxic. The use of oral fluid as an alternative specimen to blood or urine was investigated. This was through the British Roadside Impairment Test Evaluation (BRITE) project. LC-MS in combination with GC-MS was used to screen for over 50 licit and illicit drugs in 1mL of oral fluid. LC-MS-MS was then used to identify and quantitated 21 drugs of abuse and their metabolites using a similar sample size. The use of one extraction and the reliability of LC-MS proved invaluable in these projects.

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Morrison, Calum M. "Chiral and achiral analysis of benzodiazepine and anti-anginal drugs in forensic toxicology." Thesis, University of Glasgow, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.321443.

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42

Kashkary, Loay M. T. "Development of a combined DNA and drug extraction methodology for forensic toxicology application." Thesis, University of Hull, 2014. http://hydra.hull.ac.uk/resources/hull:11661.

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Biological samples recovered at crime scenes may contain unsuspected and valuable evidence, such as illicit drugs, in addition to nucleic acids. Deoxyribonucleic acid (DNA) analysis provides valuable information to identify a suspect or victim, as well as to exclude an innocent individual as the perpetrator of a crime. Identification of drugs can also be very informative for forensic investigation to determine whether a perpetrator committed a crime under the influence of illicit substances. In the field of forensic analysis, sample preparation for identifying both DNA and drugs of abuse represents a challenge due to limited sample quantity and only trace levels of target analytes present in the matrices. As a result, an analytical approach has been developed to enable the combined extraction of DNA and four amphetamines (amphetamine [AM], methamphetamine [MA], 3,4-methylenedioxyamphetamine [MDA], and 3,4-methylenedioxymethamphetamine hydrochloride [MDMA]) from a small amount of sample (50 μl) using a single extraction procedure. This study has focused on solid-phase extraction (SPE) using inorganic silica-based matrices as sorbents to facilitate such sample processing. The advantages of using inorganic silica-based monoliths are due to the simple fixation of the material in a column or within a microfluidic device, their mechanical stability with organic solvents, the availability of simple surface modifications to enable the desired chemical interaction with the target molecules, and a unique bimodal structure that allows a large surface area with minimum back pressure. A dual-phase SPE method was developed consisting of silica beads modified with octadecyl groups packed inside a luer lock adapter for amphetamine extraction coupled in series with a silica-based monolith for DNA extraction within a microfluidic system for a fully combined genetic and drug extraction system. The proposed method was effective for the extraction of the target drugs from a spiked buffer and artificial urine giving an average recovery greater than 70% and 50%, respectively, with high reproducibility (˂ 15% RSD). The limits of detection were 0.6 μg ml⁻¹ for AM and MA, 0.7 μg ml⁻¹ for MDA, and 0.8 μg ml⁻¹ for MDMA with linear calibration curves between 0.625 and 20 μg ml⁻¹. The method was also able to extract DNA from the spiked TE buffer and urine sample with average extraction efficiencies of 36% and 30%, respectively, which were successfully amplified via the polymerase chain reaction (PCR). The proposed method is not only suitable for the combined extraction of DNA and amphetamines from a limited sample size, but also reduces sample handling and potential contamination. This method could, in future, be applied to anti-doping analysis for the detection of doping agents and conducting DNA profiling as evidence to ascertain whether samples belong to the right athletes.

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González, Elera Sixto Antonio, and Elera Sixto Antonio González. "Interpretación de cromatogramas de GC-MS obtenidos a partir de hisopados de manos de manipuladores de cocaína en diversas regiones del Perú, en el Instituto de Medicina Legal y Ciencias Forenses del Ministerio Público, durante el año 2012." Bachelor's thesis, Universidad Nacional Mayor de San Marcos, 2017. http://cybertesis.unmsm.edu.pe/handle/cybertesis/6683.

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Publicación a texto completo no autorizada por el autor
Realiza el análisis de los Espectros de Masa de 293 cromatogramas obtenidos mediante un Cromatografo de Gases con Espectrómetro de masas (GC-MS) como detector, a partir de hisopados de manos provenientes de diversas regiones del Perú, detectándose en 92 (31,40 %) la presencia de cocaína y derivados tal como: cinamoil cocaína I, cinamoil cocaína II, ester de metil ecgonina, cocaetileno, ácido benzoico, benzoil cocaína, y en 33 (11,26 %) la presencia de adulterantes, tal como sigue: 25 con fenacetina (8,53%), 4 con paracetamol (1,36%), 1 con lidocaína (0,34%), 1 con endrin (0,34%) y 2 con Δ 9 - THC (Delta-9 tetra hidro cannabinol) (0,68%). Los resultados obtenidos indican las sustancias que utilizan los manipuladores de cocaína en el Perú.
Tesis de Segunda Especialidad

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Swortwood, Madeleine Jean. "Comprehensive Forensic Toxicological Analysis of Designer Drugs." FIU Digital Commons, 2013. http://digitalcommons.fiu.edu/etd/997.

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New designer drugs are constantly emerging onto the illicit drug market and it is often difficult to validate and maintain comprehensive analytical methods for accurate detection of these compounds. Generally, toxicology laboratories utilize a screening method, such as immunoassay, for the presumptive identification of drugs of abuse. When a positive result occurs, confirmatory methods, such as gas chromatography (GC) or liquid chromatography (LC) coupled with mass spectrometry (MS), are required for more sensitive and specific analyses. In recent years, the need to study the activities of these compounds in screening assays as well as to develop confirmatory techniques to detect them in biological specimens has been recognized. Severe intoxications and fatalities have been encountered with emerging designer drugs, presenting analytical challenges for detection and identification of such novel compounds. The first major task of this research was to evaluate the performance of commercially available immunoassays to determine if designer drugs were cross-reactive. The second major task was to develop and validate a confirmatory method, using LC-MS, to identify and quantify these designer drugs in biological specimens. Cross-reactivity towards the cathinone derivatives was found to be minimal. Several other phenethylamines demonstrated cross-reactivity at low concentrations, but results were consistent with those published by the assay manufacturer or as reported in the literature. Current immunoassay-based screening methods may not be ideal for presumptively identifying most designer drugs, including the “bath salts.” For this reason, an LC-MS based confirmatory method was developed for 32 compounds, including eight cathinone derivatives, with limits of quantification in the range of 1-10 ng/mL. The method was fully validated for selectivity, matrix effects, stability, recovery, precision, and accuracy. In order to compare the screening and confirmatory techniques, several human specimens were analyzed to demonstrate the importance of using a specific analytical method, such as LC-MS, to detect designer drugs in serum as immunoassays lack cross-reactivity with the novel compounds. Overall, minimal cross-reactivity was observed, highlighting the conclusion that these presumptive screens cannot detect many of the designer drugs and that a confirmatory technique, such as the LC-MS, is required for the comprehensive forensic toxicological analysis of designer drugs.

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Gonçalves, Fernando Colnago. "Identificação molecular e análise filogenética de amostras de Cannabis apreendidas pela Polícia Civil do Estado do Espírito Santo." reponame:Repositório Institucional da UFES, 2015. http://repositorio.ufes.br/handle/10/1894.

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FAPES
Popularmente conhecida como maconha, a Cannabis sativa é a mais usada de todas as drogas ilícitas e seu comércio, em conjunto com outras drogas, é uma das atividades criminosas que mais consomem recursos públicos e está intimamente associado aos homicídios. No Estado do Espírito Santo (ES), 70% dos homicídios tem relação com o tráfico de entorpecentes, apresentando atualmente o segundo maior índice dos país. A despeito da atuação policial, não existem estudos detalhados sobre plantio, distribuição e consumo de Cannabis no Brasil, de uma forma geral, sabe-se apenas que a maior parte da droga é produzida no Paraguai ou cultivada dentro do próprio país e acredita-se que o Paraguai seja responsável pelo abastecimento das regiões sul, sudeste e centro-oeste do Brasil. A identificação genética de Cannabis apreendidas pela Polícia Civil pode auxiliar na determinação geográfica de plantios e possíveis rotas do tráfico, informação essencial para a ação da polícia no combate ao tráfico de drogas. Com objetivo de caracterizar as amostras de Cannabis apreendidas pela Polícia Civil do ES e verificar correlações que pudessem indicar origens comuns, foram analisados 18 loci STR de 165 amostras oriundas de 71 dos 78 municípios do Estado. Foram encontrados 89 alelos, variando de 2 (loci A501 e 9269) a 12 alelos (locus A301). Os loci H06 e A305 apresentaram 3 alelos cada e o locus B05 apresentou 4 alelos, similar ao encontrado em amostras do Paraguai. Os dados alélicos dos loci A305, B05 e H06 sugerem que a região sudeste do Brasil pode estar sendo abastecida por Cannabis de origem Paraguaia. Também foi verificado que 4 alelos apareceram apenas nas amostras 176 e 230. A amostra 230 era proveniente de uma apreensão realizada na cidade de Aracruz, onde a Polícia verificou a ligação do proprietário com o tráfico internacional de entorpecentes, e demonstrou ser geneticamente mais próxima de amostras da Alemanha, sugerindo que sua matriz tem origem no exterior podendo, dentre outras possibilidades, ter chegado ao ES através do tráfico pela internet. Os resultados obtidos fornecem mais informações a respeito da maconha comercializada no Brasil, podendo ser utilizados em estudos futuros para elaboração de um banco de dados baseado em STR para aplicação forense.
Popularly known as marijuana, Cannabis sativa is the most used of all illicit drugs and, with other drugs, its trade is one of the criminal activities that most consume public resources and is closely related to homicides. In the Espírito Santo State (ES), 70% of homicides is related to drug trafficking, currently presenting the second highest rate in the country. Despite the police action, there is no detailed studies of planting, distribution and Cannabis consumption in Brazil, in general, we only know that most drug is produced in Paraguay or grown within the country and it is believed that Paraguay is responsible for supplying the Brazil’s south, southeast and centerwest region. Genetic analysis of Cannabis seized by the police can assist in determining, geographically, plantations and possible routes of trafficking, essential information for police’s action in drug trafficking combat. In order to characterize the Cannabis samples seized by the police at ES and verify correlations that could indicate common origins, we analyzed 18 STR loci in 165 samples from 71 of 78 municipalities in the State. We have found 89 alleles ranging from 2 (A501 loci and 9269) to 12 alleles (A301 locus). The loci H06 and A305 presented each, 3 alleles and the locus B05, 4 alleles, similar to that found in Paraguayan samples. The allelic data of loci A305, B05 and H06 suggest that Brazil 's southeast region can be being supplied by Paraguayan Cannabis. We also found four alleles that appeared only in samples 176 and 230. Sample 230 was seized in Aracruz city, where the police found owner's connection with international trafficking, and demonstrated to be genetically nearest to German samples, suggesting a foreign origin what could be explained by internet trafficking. The obtained results provide more information about marijuana’s market in Brazil and could be used in future studies to develop a STR database for forensic application.

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Toledo, Fernanda Crossi Pereira de. "Verificação do uso de cocaína por indivíduos vítimas de morte violenta na região Bragantina - SP." Universidade de São Paulo, 2004. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-13012012-143705/.

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As mortes por causas externas e o consumo de drogas são problemas crescentes nos grandes centros urbanos. No estudo foi investigado se estes fatores, também afrontam cidades de médio e pequeno porte da região Bragantina. Foram realizadas análises toxicológicas para verificar a exposição à cocaína, em amostras de cabelo e urina de indivíduos vítimas de morte violenta (n=42), submetidos à necropsia no Instituto Médico Legal de Bragança Paulista. Do total de indivíduos submetidos ao estudo, 14% apresentaram resultados positivos para cocaína. Foi possível verificar que 38% das vítimas de homicídios eram usuários de cocaína. O perfil sociodemográfico dos indivíduos vítimas de morte violenta foi: sexo masculino, branco, solteiro, faixa etária de 21-30 anos e empregados. No estudo foi constatada exposição à cocaína entre vítimas de mortes violentas ocorridas na Região Bragantina.
The deaths for externaI causes and the consumption of drugs are increasing problems in the great urban centers. In the study it was investigated if these factors also confront medium and small cities of Bragantina region. Toxicological analyses had been carried through to verify the exposure to the cocaine, in samples of hair and urine of individuaIs victims of violent death (n=42), submitted to the autopsy in the Legal Medical Institute of Bragança Paulista. Of the total of individuaIs submitted to the study, 14% had presented positive results for cocaine. It was possible to verify that 38% of homicides victims were cocaine users. The sociodemographic profile of the individuaIs victims of violent death was: male sex, white, single, 21-30 years age group and employees. In the study, exposure to the cocaine between victims of violent deaths occurred in the Bragantina Region was evidenced.

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Souza, Jéssica Priscila de. "Álcool em sangue de vítimas de morte violenta no município de São Paulo." Universidade de São Paulo, 2018. http://www.teses.usp.br/teses/disponiveis/5/5160/tde-01112018-102535/.

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O álcool é uma das substâncias psicoativas mais consumidas pela sociedade por ser de uso lícito, amplamente disponível e de baixo custo. Já foi bem estabelecido que o uso nocivo de álcool está intimamente relacionado com a violência, acarretando um número elevado de doenças relacionadas ao seu consumo, bem como com mortes violentas especialmente entre jovens. São várias as evidências científicas de sua participação nos homicídios, suicídios, violência doméstica, crimes sexuais, atropelamentos e acidentes envolvendo motoristas alcoolizados. Apesar de que esforços têm sido bem-sucedidos na redução do número de mortes atribuíveis ao álcool em vários países, lesões atribuídas ao álcool continuam sendo um problema de saúde pública. No Brasil, apesar de apresentar números expressivos de mortes violentas, ainda são poucos os estudos para nortear decisões governamentais e políticas públicas voltadas ao problema. Assim sendo, o objetivo deste estudo foi avaliar a prevalência do uso de álcool entre vítimas de morte violenta na cidade de São Paulo, através da dosagem de álcool no sangue. Foram coletadas amostras de 369 vitimas de morte violenta necropsiadas no Instituto Médico Legal do Estado de São Paulo (IML-SP). A dosagem alcoólica foi feita por cromatografia gasosa com técnica de separação por headspace. Os resultados mostram que 34.7% das vítimas haviam consumido álcool. Da amostra total 36.2% dos homens e 27.7% das mulheres haviam consumido álcool. A alcoolemia média foi 1,004 g/L nos homens e 0,767 g/L para as mulheres. Foram feitas associações entre a prevalência e a alcoolemia apresentada para homicídio, atropelamento e acidente de trânsito e diferentes causas de morte, como atropelamento, colisão, enforcamento, intoxicação, ferimentos por arma branca ou de fogo). Discute-se a aplicação desses resultados epidemiológicos para nortear a implantação de políticas públicas de prevenção
Alcohol is one of the psychoactive substances most consumed by society as it is of lawful use, widely available and inexpensive. It has been well established that the harmful use of alcohol is closely related to violence, leading to a high number of diseases related to its use, as well as violent deaths, especially among young people. There are several scientific evidences of its participation in homicides, suicides, domestic violence, sexual crimes, run-over incidents and accidents involving alcoholic drivers. Alcohol-related injuries remain a major public health problem. In Brazil, despite its significant numbers of violent deaths, there are still few studies to guide government decisions and public policies focused on the problem. Thus, the aim of this study was to evaluate the prevalence of alcohol use among victims of violent death in the country\'s largest metropolis, the city of São Paulo, by the measurement of alcohol in the blood. Samples were collected from 369 victims of necropsied violent death victims at the Legal Medical Institute of the State of São Paulo (IML-SP). The alcoholic dosage was obtained by gas chromatography with headspace separation technique. Demographic data of the victims were obtained as well as data related to the circumstances of the deaths. The results show that 34.7% of the victims had consumed alcohol. Of the total sample, 36.2% of the men and 27.7% of the women had consumed alcohol. The alcoholic dosage was, on average1,004 g/L in men e 0,767 g/L for women. Associations were tested between the blood alcoholic concentration and the type of injury (homicide, suicide, traffic-related) and methods that caused the injury like firearms, vehicle crash, hanging, intoxication, sharp weapons or other presented by the victims. We discuss the application of these epidemiological results to guide the implementation of public policies to prevent violence

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Tawil, Nádia. "Determinação de etanol em saliva através do sistema enzimático Q.E.D.® e da cromatografia em fase gasosa." Universidade de São Paulo, 2004. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-18022009-141456/.

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O uso nocivo do álcool acarreta problemas de saúde para o usuário e prejuízos na sociedade. Vários espécimes biológicos podem ser utilizados para verificar a exposição a bebidas alcoólicas. No trabalho foi investigada a utilização da saliva na determinação de etanol através das técnicas: enzimática Q.E.D. A-150 de triagem - e cromatografia em fase gasosa, após separação por aquecimento, Headspace de confirmação. O método foi padronizado, validado e aplicado em amostras de saliva provenientes de voluntários que ingeriram de maneira controlada bebida alcoólica. Em todas as amostras analisadas foi possível detectar a concentração de etanol, observando a existência de uma diferença entre os respectivos resultados das duas técnicas. Os resultados interindividuais apresentaram grande variabilidade nos mesmos tempos de coleta, apesar da ingesta equivalente de etanol. No estudo foi verificado que a saliva é uma matriz alternativa adequada para verificar a concentração de etanol em indivíduos expostos às bebidas alcoólicas.
The abuse of alcohol leads to health injury and causes damage to the society. Several biological matrices can be used to monitor exposure to alcoholic beverages. In this work, saliva was used in the determination of ethanol for both techniques: enzymatic Q.E.D. A-150 screening test -, and headspace-gas chromatography - confirmation test -. The method was developed, validated and used for the analysis of saliva samples from volunteers who ingested alcoholic beverages in a controlled schedule. Ethanol was detected and in all samples, noticing a difference between the results of both techniques. Inter-volunteers results showed high variability for the same collection times, although the amount of ethanol ingested was equivalent. These results suggest that saliva is a good option for the in field determination of ethanol in exposed individuals to alcoholic beverages.

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Pereira, Denize Duarte. "Determinação de Flunitrazepam e 7¬aminoflunitrazepam em soro por cromatografia líquida de alta eficiência acoplada à espectrometria de massa em tandem com a utilização de extração on line: aspecto forense." Universidade de São Paulo, 2005. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-29012018-154046/.

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Atualmente os benzodiazepínicos constituem o grupo de fármacos de prescrição mais consumidas em todo o mundo. Além da utilização desta classe farmacológica como fármacos de abuso, mais recentemente seu uso está associado a uma nova cultura psicodélica emergente. O termo \"club drugs\" tem sido usado para descrever estes fármacos que levam a efeitos psicodélicos e euforizantes. Acresça-se a isto à preocupante utilização destas substâncias em situações de estupro e/ou assalto, as chamadas \"drug-facilitated sexual assault\", destacando-se o flunitrazepam. Devido às pequenas doses administradas e a extensiva metabolização, a identificação do flunitrazepam e seus metabólitos torna-se dificultada em relação a outros benzodiazepínicos. O presente trabalho constitui validação de metodologia analítica que permita a correta identificação e quantificação de flunitrazepam e seu principal produto de biotransformação, o 7-aminoflunitrazepam, em soro. O método desenvolvido mostrou boa linearidade, precisão, exatidão, rendimento e capacidade de detectar os analitos mesmo em baixas concentrações, permitindo desta forma a inferência sobre a realidade dos casos onde se utiliza este fármaco sem fins terapêuticos.
Currently the benzodiazepines are one of the most consumed groups among the prescripton drugs in the world. Beside this, they have been used as drugs of abuse and more recently their use is associated with the new emerging psychodelic culture. The term \"club drugs\" has been used to describe these drugs that cause psychodelic and euphoric effects. In addition to this, there is a growing concern with the use of these substances related to \"drug-facilitated sexual assault\", among of which Flunitrazepan is pointed out as one of the most important . Due to the small doses involved in the consumption for this purpose and also the extense biotransformation, the identification of this analyte and its metabolites become more difficult than that of other benzodiazeines. This study provides an analytical validation method that enables correct identification and quantification of Flunitrazepam and its main biotransformation product, the 7-aminoflunitrazepam, in serum. The method developed demonstrates good linearity, precision, accuracy, recovery and capacity of detect the analytes, even in low concentration. Thus making possible to makes inferences regarding the reality of cases where it is used as a drug without therapeutic use.

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Alves, Sergio Rabello. "Toxicologia forense e saúde pública: desenvolvimento e avaliação de um sistema de informações como potencial ferramenta para a vigilância e monitoramento de agravos decorrentes da utilização de substâncias químicas." reponame:Repositório Institucional da FIOCRUZ, 2005. https://www.arca.fiocruz.br/handle/icict/4368.

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Um dos maiores problemas enfrentados pelas instâncias tomadoras de decisão, no que diz respeito à implementação de programas de vigilância e prevenção nestas áreas relaciona-se com a real quantificação ou dimensionamento do problema. Dentro desta fundamentação, o objetivo geral desta Tese foi desenvolver um Sistema de Informações toxicológicas forense no âmbito do Estado do Rio de Janeiro, avaliar o perfil epidemiológico (estudo descritivo) das exposições/intoxicações envolvendo a utilização de substâncias químicas, e diagnosticar/quantificar qualquer enventual fenômeno de subnotificação. (...) Destes, mais de um terço dos casos concluídos (36,96 por cento) foram considerados positivos. (...) Analgésicos obtiveram um espectro mais amplo de casos positivos (20 a 59 anos - 77,5 por cento). Em relação ao álcool, os municípios mais afetados foram Marica, Ioraí, Saquarema, Rio Bonito, Araruama, Silva Jardim, Armação de Búzios, São José do Vale do Rio Preto, Teresópolis, Sumidouro, Cordeiro e Trajano de Morais -- 22 a 49 casos: 100.000 hab. Rio de Janeiro, Niterói, Nova Iguaçu, Duque de Caxias, São João de Meriti, Mesquita, Nilópolis e Belford Roxo respondem pelos maiores prevalências relacionadas a praguicidas - 10 a 191 casos: 100.000 hab. Maiores ocorrências para Medicamentos, foram localizadas em Angra dos Reis; Itaguaí, Rio das Flores, Teresópolis e Cantagalo -- 3 a 5 casos:100.000 hab. Drogas de abuso apresentaram maiores índices de subnotificação em relação ao Sistema Nacional de Informações sobre Mortalidade - SIM e Sistema Nacional de Informações Tóxicofarmacológicas - SINITOX (99,40 por cento e 100,00 por cento, respectivamente). (...) Praguicidas foi a categoria de substâncias que apresentaram o menor grau de não registros SIM (12,93 por cento) e SINITOX (69,09 por cento).

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