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Gerhard, Daniel [Verfasser]. "Simultaneous small sample inference based on profile likelihood / Daniel Gerhard." Hannover : Technische Informationsbibliothek und Universitätsbibliothek Hannover, 2010. http://d-nb.info/1008373680/34.
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Haines, Ross. "Simultaneous reconstruction of spatial frequency fields and field sample locations." Thesis, University of Oxford, 2016. https://ora.ox.ac.uk/objects/uuid:aa35073d-003b-4939-bf0e-8348243871b7.
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Classically, spatial smoothing methods such as kriging estimate smooth interpolating fields for features measured at well-located points. In this thesis, we make a simultaneous reconstruction of interpolating spatial fields and measurement locations. We give models, and sample-based Bayesian inference, for estimating locations of dialect samples on a map of England. The method exploits dialect-based spellings to locate these samples. The data are feature vectors extracted from written dialect samples. Just a fraction of the feature vectors ('anchors') have an associated spatial location. When coupled to a prior for the smoothly varying feature field, and the anchor texts, the unlocated feature vectors are jointly informative of their own location and the feature fields. The dataset is large, but sparse, since a given word has a large number of variant spellings which may appear in just a few documents. We report an analysis including Bayesian model fitting and validation on a large and representative subset of the data. The thesis has two main aims - to provide statistical tools for the linguists who collected the data, and to meet the computational and inferential challenge of simultaneously locating large numbers of feature vectors. The results presented in this thesis show that we have largely succeeded in meeting these challenges.
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Anderson, Andrew D. (Andrew David). "Recovering sample diversity in Rao-Blackwellized particle filters for simultaneous localization and mapping." Thesis, Massachusetts Institute of Technology, 2006. http://hdl.handle.net/1721.1/36174.
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Thesis (S.M.)--Massachusetts Institute of Technology, Dept. of Aeronautics and Astronautics, 2006.Includes bibliographical references (p. 105-109).
This thesis considers possible solutions to sample impoverishment, a well-known failure mode of the Rao-Blackwellized particle filter (RBPF) in simultaneous localization and mapping (SLAMI) situations that arises when precise feature measurements yield a limited perceptual distribution relative to a motion-based proposal distribution. One set of solutions propagates particles according to a more advanced proposal distribution that includes measurement information. Other methods recover lost sample diversity by resampling particles according to a continuous distribution formed by regularization kernels. Several advanced proposals and kernel shaping regularization methods are considered based on the RBPF and tested in a Monte Carlo simulation involving an agent traveling in an environment and observing uncertain landmarks. RMS error of range-bearing feature measurements was reduced to evaluate performance during proposal-perceptual distribution mismatch. A severe loss in accuracy due to sample impoverishment is seen in the standard RBPF at a measurement range RMS error of 0.001 m in a 10 m x 10 m environment.
(cont.) Results reveal a robust and accurate solution to sample impoverishment in an RBPF with an added fixed-variance regularization algorithm. This algorithm produced an average 0.05 m improvement in agent pose CEP over standard FastSLAM 1.0 and a 0.1 m improvement over an RBPF that includes feature observations in formulation of a proposal distribution. This algorithm is then evaluated in an actual SLAM environment with data from a Swiss Ranger LIDAR measurement device and compared alongside an extended Kalman filter (EKF) based SLAM algorithm. Pose error is immediately recovered in cases of a 1.4 m error in initial agent uncertainty using the improved FastSLAM algorithm, and it continues to maintain an average 0.75 m improvement over an EKF in pose CEP through the scenario.
by Andrew D. Anderson.
S.M.
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Khalaf, Lynda. "Simulation based finite and large sample inference methods in seemingly unrelated regressions and simultaneous equations." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1997. http://www.collectionscanada.ca/obj/s4/f2/dsk1/tape11/PQDD_0008/NQ38813.pdf.
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Berdugo, Albert. "ADVANCED DISTRIBUTED WIDEBAND DATA ACQUISITION SYSTEM." International Foundation for Telemetering, 2005. http://hdl.handle.net/10150/604918.
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ITC/USA 2005 Conference Proceedings / The Forty-First Annual International Telemetering Conference and Technical Exhibition / October 24-27, 2005 / Riviera Hotel & Convention Center, Las Vegas, NevadaWideband data acquisition units have been used as part of an instrumentation system for several decades. Historically, these units operated asynchronously from each other, and from the rest of the instrumentation system when installed on the same test vehicle. When many wideband units are required to slave their formats or sampling rate to the test vehicle’s event of interest such as external computer event clock, radar, or laser pulse train; few solutions were available. Additionally, a single test vehicle may use ten to thirty wideband units operating at up to 20 Mbps each. Such systems present a challenge to the instrumentation engineers to synchronize, transmit safety of flight information, and record. This paper will examine a distributed wideband data acquisition system in which each acquisition unit operates under its own data rate and format, yet remains fully synchronized to an external fixed or variable simultaneous sampling rate to provide total system coherency. The system aggregate rate can be as low as a few Mbps to as high as 1 Gbps. Data acquired from the acquisition units is further multiplexed per IRIG-106 chapter 10 using distributed data multiplexers for recording.
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Rinker, Brett A. "A single-sided access simultaneous solution of acoustic wave speed and sample thickness for isotropic materials of plate-type geometry." Diss., Columbia, Mo. : University of Missouri-Columbia, 2006. http://hdl.handle.net/10355/4585.
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Thesis (M.S.)--University of Missouri-Columbia, 2006.The entire dissertation/thesis text is included in the research.pdf file; the official abstract appears in the short.pdf file (which also appears in the research.pdf); a non-technical general description, or public abstract, appears in the public.pdf file. Title from title screen of research.pdf file (viewed on April 17, 2009) Vita. Includes bibliographical references.
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Wang, Yinna. "Efficient Stepwise Procedures for Minimum Effective Dose Under Heteroscedasticity." Bowling Green State University / OhioLINK, 2012. http://rave.ohiolink.edu/etdc/view?acc_num=bgsu1339037272.
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Portela, Milena Moura Fé Araújo. "Controle restrito de estímulos em autistas: avaliação de um procedimento de Resposta de Observação Diferencial e estímulos com diferenças críticas." Pontifícia Universidade Católica de São Paulo, 2014. https://tede2.pucsp.br/handle/handle/16731.
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Previous issue date: 2014-03-27The objective of this work was to investigate whether the procedure of Differential Observing Responses (DOR) used in a training with words as stimuli with critical differences could reduce/eliminate the restricted stimulus control in autistic participants. For this, six children diagnosed with autistic disorder underwent tasks of matching-tosample simultaneous (SMTS). Three of them participated in the control group and three in the experimental group. There were used in attempts to SMTS, three sets of words: BO set (good, good, box), PA set (par, peace, father) and ME set (month, my, honey). The attempts with critical differences included stimuli of a same set and the ones with multiple differences had stimuli of the three sets of words. Children in the experimental group were submitted to seven phases: initial evaluation of restricted stimuli control, base line 1, DOR condition, baseline 2, the generalization test, final evaluation of restricted stimulus control and follow-up. Children in the control group were only submitted to the phases of the initial evaluation, base line 1 and base line 2. For two participants in the experimental group, a delineation of multiple base line among participants was used. For the other participant in the experimental group, it was used a procedure of multiple base line among sets. The analysis of the results identified that the answer under restricted stimulus control of the experimental participants was reduced. This result was observed even with the return to the base line (reversal). In addition, it was achieved a high rate of correct answers on the generalization test, in which the stimuli were changed position. Another significant result was achieved in reapplying the test one month after the end of the procedure; the results of the participants remained accurate, indicating generality in time regarding the responding reduction under strict control in tasks of SMTS
A presente pesquisa teve como objetivo investigar se o procedimento de Resposta de Observação Diferencial (DOR) utilizado em um treino com palavras como estímulos com diferenças críticas era capaz de reduzir/eliminar o controle restrito de estímulos em participantes autistas. Para isso, seis crianças diagnosticadas com o transtorno autista foram submetidas a tarefas de matching-to-sample simultâneo (SMTS). Três delas participaram do grupo controle e três do grupo experimental. Foram utilizadas nas tentativas de SMTS três conjuntos de palavras: BO (boa, bom, box), PA (par, paz pai) e ME (mes, meu, mel). As tentativas com diferenças críticas continham estímulos de um mesmo conjunto e as com diferenças múltiplas, dos três conjuntos de palavras. As crianças do grupo experimental foram submetidas a sete fases: avaliação inicial do controle restrito de estímulos, linha de base 1, condição DOR, linha de base 2, teste de generalização, avaliação final do controle restrito de estímulo e follow-up. As crianças do grupo controle passaram apenas pelas fases de avaliação inicial e linhas de base 1 e 2. Para dois participantes do grupo experimental foi utilizado ainda um delineamento de linha de base múltipla entre participantes. Para o outro participante do grupo experimental utilizou-se um procedimento de linha de base múltipla entre conjuntos. A análise dos resultados permitiu identificar que o responder sob controle restrito de estímulos dos participantes experimentais foi reduzido. Esse resultado manteve-se mesmo com o retorno à linha de base (reversão). Além disso, foi obtido um alto escore de acertos no teste de generalização, no qual os estímulos tiveram suas posições recombinadas. Outro resultado relevante foi obtido na reaplicação desse teste um mês após o término do procedimento. Os resultados dos participantes mantiveram-se precisos, indicando generalidade no tempo quanto à redução do responder sob controle restrito em tarefas de SMTS
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Gouveia, Carla Alexandra Pereira. "Simultaneous quantification of morphine and cocaine in hair samples by gas chromatography-mass spectrometry." Dissertação, Faculdade de Medicina da Universidade do Porto, 2011. http://hdl.handle.net/10216/63790.
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Gouveia, Carla Alexandra Pereira. "Simultaneous quantification of morphine and cocaine in hair samples by gas chromatography-mass spectrometry." Master's thesis, Faculdade de Medicina da Universidade do Porto, 2011. http://hdl.handle.net/10216/63790.
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Kim, Hang Joon. "The Generalized Multiset Sampler: Theory and Its Application." The Ohio State University, 2012. http://rave.ohiolink.edu/etdc/view?acc_num=osu1338332071.
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Valeinis, Janis. "Confidence bands for structural relationship models." Doctoral thesis, [S.l.] : [s.n.], 2007. http://webdoc.sub.gwdg.de/diss/2007/valeinis.
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Gray, Nicholas. "Bioanalysis of small molecule pharmaceuticals : simultaneous determination in biological fluid samples from multiple species by the management of matrix effects." Thesis, Northumbria University, 2011. http://nrl.northumbria.ac.uk/709/.
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A strategy is described for method evaluation to manage the influence of endogenous compounds to induce bias in pharmaceutical quantification from blood samples of different animal species resulting from ionisation matrix effects. The approach introduces the possibility of simultaneous cross animal species calibration for ethical reasons using a simple indicative test, which also rapidly demonstrates the utility of a test assay in other matrices. A quantitative Turboflow LC-MS/MS assay was evaluated using samples prepared in species matched controlled matrices with deuterated internal standardisation. The method was subsequently tested to assess the analysis of samples from multiple animal species using calibration samples from a single matrix origin. The object of this was to enable the substitution of analytical control samples in rodent plasma, reducing the plasma volume required, therefore the number of rodents used indirectly to support development studies. The method was unsuccessful due to concentration bias in identically prepared test samples. The bias origin was investigated using a fixed ratio solution of the analyte and its deuterated analogue with matrix test aliquots. The investigation identified non equivalent relative ionisation efficiency between compounds. The ratio method is proposed as an evaluation strategy for matrix effects causing non-equivalent response ratios. The origin of this deviation was identified using a post column standard infusion test highlighting a region of ionisation suppression co-eluting with the analyte. Full scan acquisition analysis revealed co-elution of endogenous glycerophospholipids. The relative expression of these compounds between species was investigated, employing a precursor ion scanning method of a common product ion indicative of phosphotidyl choline compounds; the human diversity was also investigated. Distribution was found to differ between animal species, which was further tested by construction of a model using partial least squares regression which correctly identified the species origin of all non-primate species tested. The mechanism of differentiation between compound and deuterated analogue by endogenous phosphotidyl choline was proposed as micellar phase equilibrium following elution from the HPLC column. A new Turboflow LC-MS/MS assay was optimised with attention to the resolution of glycerophospholipid interferences and retested for applicability between species. It was simultaneously applied to the analysis of small volume whole blood samples via dried blood spots on filter paper. Precision and bias were acceptable for the analysis of rat and mouse samples using human control plasma. Analysis of incurred ex-vivo samples from rats was successful in demonstrating equivalence between calibration sources.
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Klassen, Cherie Leanne. "The development and application of an electron-capture gas chromatographic assay procedure for the simultaneous determination of sertraline and N-desmethylsertraline in biological samples." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1999. http://www.collectionscanada.ca/obj/s4/f2/dsk2/ftp01/MQ40071.pdf.
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Šerkšnas, Juozas. "Regimųjų vaizdų pasukimo mintyse tyrimas, pateikiant juos vienu metu ir nuosekliai." Master's thesis, Lithuanian Academic Libraries Network (LABT), 2010. http://vddb.laba.lt/obj/LT-eLABa-0001:E.02~2007~D_20101125_183216-64428.
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Darbo tikslas – atskleisti figūrų, pateikiamų vienu metu ir nuosekliai, sukimo mintyse ypatumus naudojant tapatumo įvertinimo užduotį. Tiriamieji (32 studentai) atliko tapatumo vertinimo užduotį, kur jiems vienu metu bei nuosekliai (arba atvirkštine tvarka) buvo pateikiamos vienodų arba skirtingų netaisyklingų daugiakampių poros. Stimulai buvo rodomi 100ms vienalaikio pateikimo atveju, esant nuosekliam pateikimui 50ms ir 50ms. Tiriamieji turėjo atsakyti, ar figūros vienodos (nepaisant pasukimo kampo), ar skirtingos. Buvo matuojamas reakcijos laikas bei teisingų atsakymų skaičius. Nustatyta, kad nepasuktos viena kitos atžvilgiu vienodos figūros atpažįstamos tiksliau bei greičiau nei pasuktos bet kokiu kampu. Tiek vienalaikio, tiek nuoseklaus figūrų pateikimo atveju tiesinė reakcijos laiko priklausomybė nuo figūrų tarpusavio pasukimo kampo nenustatyta. Tiek vienodos, tiek skirtingos figūros nuoseklaus pateikimo atveju atpažįstamos tiksliau nei vienalaikio, o reakcijos laikas, vertinant tiek vienodas, tiek skirtingas figūras, trumpesnis vienalaikio pateikimo atveju nei nuoseklaus. Vyrų ir moterų vienodų figūrų atpažinimo tikslumas nesiskiria, bet vyrų reakcijos laikas trumpesnis nei moterų.The purpose of this study was to examine mental rotation of simultaneously and successively presented figures. 32 students performed same – different task in which the pairs of the same or different irregular polygons were presented simultaneously and successively or vice versa. Stimuli were presented briefly – for 100 ms when presented simultaneously and 50 ms and 50 ms when presented successively. The subjects had to answer whether the two figures were the same or different. Response time and performance accuracy were recorded. The results of the experiment showed that not rotated figures were identified faster and more accurately than those rotated at any angle. The increase in reaction time as a linear function of the angle of rotation was not found (either under simultaneous presentation or under successive one).The same figures as well as the different ones were identified more accurately when presented successively than simultaneously and the response time was shorter under simultaneous presentation than under successive one. The accuracy of men and women did not differ, but men outperformed women by response time.
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Wu, Debo [Verfasser], Thomas [Akademischer Betreuer] Pichler, and Andrea [Akademischer Betreuer] Koschinsky. "Optimization of methodology for the simultaneous speciation of inorganic As, Sb and Se in fluid samples by sector-field ICP-MS coupled to HPLC / Debo Wu. Gutachter: Thomas Pichler ; Andrea Koschinsky. Betreuer: Thomas Pichler." Bremen : Staats- und Universitätsbibliothek Bremen, 2015. http://d-nb.info/1075609313/34.
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Swiha, Stéphanie. "Optimisation du suivi de l'exposition aux hydrocarbures aromatiques polycycliques pendant la grossesse avec le développement et la validation de méthodes analytiques et biologiques Analysis of polycyclic aromatic hydrocarbons in human biological samples Development of an analytical method for the simultaneous quantitation of 24 regulated Polycyclic Aromatic Hydrocarbons (PAHs) in maternal and umbilical cord sera Validation of the analytical procedure for the determination of 22 regulated polycyclic aromatic hydrocarbons in maternal and umbilical cord sera." Thesis, Sorbonne Paris Cité, 2019. http://www.theses.fr/2019USPCB020.
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Les Hydrocarbures Aromatiques Polycycliques (HAP) sont principalement émis par les activités humaines et représentent l'un des principaux groupes de polluants dans l'air, les sols, les eaux et les aliments. Par conséquent, ils font l'objet d'une surveillance atmosphérique, et alimentaire. Cette étude s'attache au cas particulier de la femme enceinte et son fœtus. En effet, l'exposition pendant la grossesse est à l'origine de malformations fœtales, de prématurité et de troubles pouvant survenir ensuite chez l'enfant mais aussi chez l'adulte. À ce jour, seuls quelques HAP réglementés par l'environnement ont été recherchés et quantifiés dans le sang maternel ou le sang de cordon ombilical. De plus, les données sur les performances analytiques sont souvent manquantes. Ainsi ce projet vise pour la première fois en France à développer et valider des méthodes analytiques et biologiques pour la surveillance de l'exposition aux HAP durant la grossesse. Dans une première partie, la quantification simultanée des 24 HAP réglementés dans les sérums de sang maternel et de sang de cordon ombilical a été développée. Tout d'abord, l'analyse des 24 HAP par chromatographie en phase liquide et par détections UV et fluorescence (HPLC-UV-FD) et par chromatographie en phase gazeuse couplée à la spectrométrie de masse (GC-MS) a été optimisée. Le prétraitement des échantillons de sérum a ensuite été développé. La précipitation des protéines présentes dans le sérum a été optimisée avec un plan d'expérience afin d'interrompre toutes les interactions entre les protéines et les HAP. Un protocole d'extraction sur phase solide (SPE), avec un supportt à base de silice greffée C18, a ensuite été optimisé pour extraire et concentrer les HAP. Pour améliorer les facteurs d'enrichissement, les fractions d'élution de SPE ont ensuite été évaporées et 2 approches ont été évaluées: une évaporation totale ou partielle (méthode "dernière goutte"). Le protocole analytique final impliquant la préparation d'échantillon suivi par l'analyse en HPLC-UV-FD ou GC-MS a été validé avec succès à partir d'un mélange de sérums maternels dopés et un mélange de sérums dopés provenant de sangs de cordons ombilicaux avec l'approche des profils d'exactitude. Ensuite, des échantillons de sérum provenant de sang maternel et de sang de cordon ombilical ont été analysés par HPLC-UV-FD et GC-MS. Enfin, les méthodes analytiques développées précédemment ont été utilisées pour l'étude du transfert placentaire des HAP avec le modèle de perfusion du cotylédons humains ex vivo. Les perfusions ont été réalisées pour la première fois avec un mélange de 14 HAP (concentration totale : 1 microM) et leur transfert placentaire a été démontré. De plus, des cultures cellulaires de trophoblastes humains exposées avec ce mélange de 14 HAP (concentration totale : 1 microM) ont été réalisées pour évaluer l'impact de l'exposition aux HAP sur les fonctions placentaires. Le dysfonctionnement de certaines fonctions placentaires telles que la fusion et la différentiation des trophoblastes, les fonctions endocrines et les fonctions de détoxificationsPolycyclic Aromatic Hydrocarbons (PAHs) are mainly emitted by human activities and are one of the main pollutant groups in air, soils, waters, and food. Therefore, they are subject to atmospheric, environmental and food monitoring. This study focuses on the particular case of exposure of pregnant women and their fetus, which are at risks. Indeed, PAH exposure can lead to fetal malformations, prematurity and even disorders in children and adult. To date, only a few PAHs regulated by US-EPA were searched and quantified in maternal or umbilical cord blood. Moreover, analytical performance data are often lacking. Hence, this study aims for the first time in France, at developing analytical and biological methods for the monitoring of PAH exposure during pregnancy. In a first part, the simultaneous determination of the 24 regulated PAHs in sera from maternal and umbilical cord bloods was developed. First, the analysis of the 24 PAHs by liquid chromatography and UV and fluorescence detections (HPLC-UV-FD) and by gas chromatography hyphenated to mass spectrometry (GC-MS) were optimized. The sample pretreatment of the plasma samples was next developed. The precipitation of the proteins present in the plasma was optimized with a Design of Experiment to disrupt all the interactions between them and the PAHs. A solid phase extraction (SPE) protocol, with a C18-based sorbent, was next optimized to extract and concentrate the PAHs. To improve the enrichment factors, the elution SPE fractions were next evaporated and 2 approaches were evaluated: a total or a partial evaporation ("last drop" method). The final analytical protocol involving the sample pretreatment followed by HPLC-UV-FD or GC-MS was successfully validated with spiked pooled sera from maternal and umbilical cord bloods with the accuracy profile approach. Then, sera samples from maternal and umbilical cord bloods were analyzed by LC/UV-FD and GC/MS. Finally, the previously developed analytical methods were used for a study with the ex vivo human cotyledon perfusion model. Perfusions were carried out for the first time with a mix of 14 US-EPA PAHs and their placental transfer was demonstrated. In addition, human trophoblast cell cultures with 1 µM with 14 US-EPA PAHs were carried out to evaluate the impact of PAH exposure on placental functions. The dysfunction of certain placental functions such as trophoblast fusion and differentiation, endocrine functions and detoxification functions was demonstrated
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Larabi, Islam Amine. "Nouveaux produits de synthèse : analyse, consommation et métabolisme ; Applications cliniques et médicolégales Rapid and simultaneous screening of new psychoactive substances and conventional drugs of abuse. A comparative study of Biochip Array Technology versus LC-MS/MS in whole blood and urine Development of a sensitive untargeted liquid chromatography– high resolution mass spectrometry screening devoted to hair analysis through a shared MS2 spectra database: A step toward early detection of new psychoactive substances Validation of an UPLC-MS/MS method for the determination of sixteen synthetic cannabinoids in human hair. Application to document chronic use of JWH-122 following a non-fatal overdose Development and validation of liquid chromatography-tandem mass spectrometry targeted screening of 16 fentanyl analogs and U-47700 in hair: Application to 137 authentic samples Prevalence and Surveillance of Synthetic Cathinones Use by Hair Analysis: An Update Review Prevalence of New Psychoactive Substances(NPS) and conventional drugs of abuse (DOA) in high risk populations from Paris(France) and its suburbs A cross sectional study by hair testing(2012–2017) Evaluation of drug abuse by hair analysis and self-reported use among MSM under PrEP: Results from a sub-study of the ANRS-IPERGAY trial. Hair testing for 3‑fluorofentanyl, furanylfentanyl, methoxyacetylfentanyl, carfentanil, acetylfentanyl and fentanyl by LC–MS/MS after unintentional overdose Drug‐facilitated sexual assault (DFSA) involving 4‐methylethcathinone (4‐MEC),3,4‐Methylenedioxypyrovalerone (MDPV), and doxylamine highlighted by hair analysis Metabolic Profiling of Deschloro-N-ethyl-ketamine (O-PCE) and identification of new target metabolites in urine and hair using human liver microsomes and high-resolution accurate mass spectrometry." Thesis, université Paris-Saclay, 2020. http://www.theses.fr/2020UPASL029.
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L’objectif de ce travail a été de développer deux approches analytiques dédiées à l’analyse toxicologique des nouveaux produits de synthèse (NPS) dans différentes matrices biologiques (sang, urine et cheveux). La première est basée sur le criblage non ciblé par chimiluminescence sur biopuces et chromatographie liquide couplée à la spectrométrie de masse haute résolution (LC-HRMS) et la deuxième correspond à un criblage ciblé par spectrométrie de masse en tandem (LC-MS/MS). Ces deux approches ont ensuite été appliquées dans des études observationnelles pour évaluer la consommation de NPS dans des populations à risques de surdosage, de pharmacodépendance ou de soumission chimique dans un contexte clinique ou médico-judiciaire.La dernière partie a été consacrée au développement d’un nouvel outil analytique de traitement des données issues de la LC-HRMS qui a permis d’étudier le métabolisme de 9 NPS in vitro sur des cultures de microsomes du foie humain (HLM) et in vivo sur des échantillons biologiques d’usagers de ces drogues. Cette dernière approche a permis la création d’une bibliothèque de spectres de haute résolution composée de 228 métabolites dont certains ont été proposés comme marqueurs pertinents d’exposition aux NPS dont ils sont issus.Ce travail a été concrétisé par la rédaction de 10 publications scientifiques et a permis d’initier plusieurs collaborations pluridisciplinairesThe aim of the present work was to develop two analytical approaches dedicated to the analysis of new psychoactive substances in different biological matrices (blood, urine and hair). The first approach is based on untargeted screening by both biochip array technology chemiluminescence assay and liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS) and the second corresponds to a targeted screening by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). These two approaches were then applied in observational studies to assess the consumption of NPS in high risk populations (overdose, drug abuse, drug facilitated crimes) in clinical and forensic settings. The last part of the work was devoted to the development of a new analytical tool for LC-HRMS data processing which made it possible to study the metabolism of 9 NPS In vitro on human liver microsomes (HLM) and In vivo in biological samples from drug users. This approach has enabled the creation of HRMS spectral library containing 228 metabolites, some of which have been proposed as relevant markers of NPS exposure.This work has resulted on 10 scientific publications and allowed to initiate many multidisciplinary collaborations
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Moreira, Ana Sofia Pereira. "Study of modifications induced by thermal and oxidative treatment in oligo and polysaccharides of coffee by mass spectrometry." Doctoral thesis, Universidade de Aveiro, 2016. http://hdl.handle.net/10773/17074.
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Doutoramento em BioquímicaOs polissacarídeos são os componentes maioritários dos grãos de café verde e torrado e da bebida de café. Os mais abundantes são as galactomananas, seguindo-se as arabinogalactanas. Durante o processo de torra, as galactomananas e arabinogalactanas sofrem modificações estruturais, as quais estão longe de estar completamente elucidadas devido à sua diversidade e à complexidade estrutural dos compostos formados. Durante o processo de torra, as galactomananas e arabinogalactanas reagem com proteínas, ácidos clorogénicos e sacarose, originando compostos castanhos de alto peso molecular contendo nitrogénio, designados de melanoidinas. As melanoidinas do café apresentam diversas atividades biológicas e efeitos benéficos para a saúde. No entanto, a sua estrutura exata e os mecanismos envolvidos na sua formação permanecem desconhecidos, bem como a relação estrutura-atividade biológica. A utilização de sistemas modelo e a análise por espectrometria de massa permitem obter uma visão global e, simultaneamente, detalhada das modificações estruturais nos polissacarídeos do café promovidas pela torra, contribuindo para a elucidação das estruturas e mecanismos de formação das melanoidinas. Com base nesta tese, oligossacarídeos estruturalmente relacionados com a cadeia principal das galactomananas, (β1→4)-Dmanotriose (Man3), e as cadeias laterais das arabinogalactanas, (α1→5)-Larabinotriose (Ara3), isoladamente ou em misturas com ácido 5-Ocafeoilquínico (5-CQA), o ácido clorogénico mais abundante nos grãos de café verde, e péptidos compostos por tirosina e leucina, usados como modelos das proteínas, foram sujeitos a tratamento térmico a seco, mimetizando o processo de torra. A oxidação induzida por radicais hidroxilo (HO•) foi também estudada, uma vez que estes radicais parecem estar envolvidos na modificação dos polissacarídeos durante a torra. A identificação das modificações estruturais induzidas por tratamento térmico e oxidativo dos compostos modelo foi feita por estratégias analíticas baseadas principalmente em espectrometria de massa, mas também em cromatografia líquida. A cromatografia de gás foi usada na análise de açúcares neutros e ligações glicosídicas. Para validar as conclusões obtidas com os compostos modelo, foram também analisadas amostras de polissacarídeos do café obtidas a partir de resíduo de café e café instantâneo. Os resultados obtidos a partir dos oligossacarídeos modelo quando submetidos a tratamento térmico (seco), assim como à oxidação induzida por HO• (em solução), indicam a ocorrência de despolimerização, o que está de acordo com estudos anteriores que reportam a despolimerização das galactomananas e arabinogalactanas do café durante a torra. Foram ainda identificados outros compostos resultantes da quebra do anel de açúcares formados durante o tratamento térmico e oxidativo da Ara3. Por outro lado, o tratamento térmico a seco dos oligossacarídeos modelo (individualmente ou quando misturados) promoveu a formação de oligossacarídeos com um maior grau de polimerização, e também polissacarídeos com novos tipos de ligações glicosídicas, evidenciando a ocorrência de polimerização através reações de transglicosilação não enzimática induzidas por tratamento térmico a seco. As reações de transglicosilação induzidas por tratamento térmico a seco podem ocorrer entre resíduos de açúcares provenientes da mesma origem, mas também de origens diferentes com formação de estruturas híbridas, contendo arabinose e manose como observado nos casos dos compostos modelo usados. Os resultados obtidos a partir de amostras do resíduo de café e de café instantâneo sugerem a presença de polissacarídeos híbridos nestas amostras de café processado, corroborando a ocorrência de transglicosilação durante o processo de torra. Além disso, o estudo de misturas contendo diferentes proporções de cada oligossacarídeo modelo, mimetizando regiões do grão de café com composição distinta em polissacarídeos, sujeitos a diferentes períodos de tratamento térmico, permitiu inferir que diferentes estruturas híbridas e não híbridas podem ser formadas a partir das arabinogalactanas e galactomananas, dependendo da sua distribuição nas paredes celulares do grão e das condições de torra. Estes resultados podem explicar a heterogeneidade de estruturas de melanoidinas formadas durante a torra do café. Os resultados obtidos a partir de misturas modelo contendo um oligossacarídeo (Ara3 ou Man3) e 5-CQA sujeitas a tratamento térmico a seco, assim como de amostras provenientes do resíduo de café, mostraram a formação de compostos híbridos compostos por moléculas de CQA ligadas covalentemente a um número variável de resíduos de açúcar. Além disso, os resultados obtidos a partir da mistura contendo Man3 e 5-CQA mostraram que o CQA atua como catalisador das reações de transglicosilação. Por outro lado, nas misturas modelo contendo um péptido, mesmo contendo também 5-CQA e sujeitas ao mesmo tratamento, observou-se uma diminuição na extensão das reações transglicosilação. Este resultado pode explicar a baixa extensão das reações de transglicosilação não enzimáticas durante a torra nas regiões do grão de café mais ricas em proteínas, apesar dos polissacarídeos serem os componentes maioritários dos grãos de café. A diminuição das reações de transglicosilação na presença de péptidos/proteínas pode dever-se ao facto de os resíduos de açúcares redutores reagirem preferencialmente com os grupos amina de péptidos/proteínas por reação de Maillard, diminuindo o número de resíduos de açúcares redutores disponíveis para as reações de transglicosilação. Além dos compostos já descritos, uma diversidade de outros compostos foram formados a partir dos sistemas modelo, nomeadamente derivados de desidratação formados durante o tratamento térmico a seco. Em conclusão, a tipificação das modificações estruturais promovidas pela torra nos polissacarídeos do café abre o caminho para a compreensão dos mecanismos de formação das melanoidinas e da relação estrutura-atividade destes compostos.
Polysaccharides are the major components of green and roasted coffee beans, and coffee brew. The most abundant ones are galactomannans, followed by arabinogalactans. During the roasting process, galactomannans and arabinogalactans undergo structural modifications that are far to be completely elucidated due to their diversity and complexity of the compounds formed. During the roasting process, galactomannans and arabinogalactans react with proteins, chlorogenic acids, and sucrose, originating high molecular weight brown compounds containing nitrogen, known as melanoidins. Several biological activities and beneficial health effects have been attributed to coffee melanoidins. However, their exact structures and the mechanisms involved in their formation remain unknown, as well as the structure-biological activity relationship. The use of model systems and mass spectrometry analysis allow to obtain an overall view and, simultaneously, detailed, of the structural modifications in coffee polysaccharides promoted by roasting, contributing to the elucidation of the structures and formation mechanisms of melanoidins. Based on this thesis, oligosaccharides structurally related to the backbone of galactomannans, (β1→4)-D-mannotriose, and the side chains of arabinogalactans, (α1→5)-Larabinotriose, alone or in mixtures with 5-O-caffeoylquinic acid, the most abundant chlorogenic acid in green coffee beans, and dipeptides composed by tyrosine and leucine, used as models of proteins, were submitted to dry thermal treatments, mimicking the coffee roasting process. The oxidation induced by hydroxyl radicals (HO•) was also studied, since these radicals seem to be involved in the modification of the polysaccharides during roasting. The identification of the structural modifications induced by thermal and oxidative treatment of the model compounds was performed mostly by mass spectrometry-based analytical strategies, but also using liquid chromatography. Gas chromatography was used in the analysis of neutral sugars and glycosidic linkages. To validate the conclusions achieved with the model compounds, coffee polysaccharide samples obtained from spent coffee grounds and instant coffee were also analysed. The results obtained from the model oligosaccharides when submitted to thermal treatment (dry) or oxidation induced by HO• (in solution) indicate the occurrence of depolymerization, which is in line with previous studies reporting the depolymerization of coffee galactomannans and arabinogalactans during roasting. Compounds resulting from sugar ring cleavage were also formed during thermal treatment and oxidative treatment of Ara3. On the other hand, the dry thermal treatment of the model oligosaccharides (alone or when mixed) promoted the formation of oligosaccharides with a higher degree of polymerization, and also polysaccharides with new type of glycosidic linkages, evidencing the occurrence of polymerization via non-enzymatic transglycosylation reactions induced by dry thermal treatment. The transglycosylation reactions induced by dry thermal treatment can occur between sugar residues from the same origin, but also of different origins, with formation of hybrid structures, containing arabinose and mannose in the case of the model compounds used. The results obtained from spent coffee grounds and instant coffee samples suggest the presence of hybrid polysaccharides in these processed coffee samples, corroborating the occurrence of transglycosylation during the roasting process. Furthermore, the study of mixtures containing different proportions of each model oligosaccharide, mimicking coffee bean regions with distinct polysaccharide composition, subjected to different periods of thermal treatment, allowed to infer that different hybrid and non-hybrid structures may be formed from arabinogalactans and galactomannans, depending on their distribution in the bean cell walls and on roasting conditions. These results may explain the heterogeneity of melanoidins structures formed during coffee roasting. The results obtained from model mixtures containing an oligosaccharide (Ara3 or Man3) and 5-CQA and subjected to dry thermal treatment, as well as samples derived from spent coffee grounds, showed the formation of hybrid compounds composed by CQA molecules covalently linked to a variable number of sugar residues. Moreover, the results obtained from the mixture containing Man3 and 5-CQA showed that CQA acts as catalyst of transglycosylation reactions. On the other hand, in the model mixtures containing a peptide, even if containing 5-CQA and subjected to the same treatment, it was observed a decrease in the extent of transglycosylation reactions. This outcome can explain the low extent of non-enzymatic transglycosylation reactions during roasting in coffee bean regions enriched in proteins, although polysaccharides are the major components of the coffee beans. The decrease of transglycosylation reactions in the presence of peptides/proteins can be related with the preferential reactivity of reducing residues with the amino groups of peptides/proteins by Maillard reaction, decreasing the number of reducing residues available to be directly involved in the transglycosylation reactions. In addition to the compounds already described, a diversity of other compounds were formed from model systems, namely dehydrated derivatives formed during dry thermal treatment. In conclusion, the identification of the structural modifications in coffee polysaccharides promoted by roasting pave the way to the understanding of the mechanisms of formation of melanoidins and structure-activity relationship of these compounds.
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Huang, Pei-Li, and 黃佩莉. "Simultaneous determination ofaripiprazole and dehydroaripiprazole in human plasma by field-amplified sample stacking and capillary electrophoresis." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/87439986790180768096.
Full textAbstract:
碩士高雄醫學大學
藥學研究所
97
A sensitive high performance capillary zone electrophoresis (CZE) combining on-column field-amplified sample stacking (FASS) has been developed for simultaneous determination of aripiprazole and its active metabolite, dehydroaripiprazole, in human plasma. A sample pretreatment by means of liquid-liquid extraction (diethylether) with subsequent quantitation by FASS-CZE was used. The separation of aripiprazole and dehydroaripiprazole was performed using a background electrolyte containing 150 mM phosphate buffer (pH 3.5) with 40% methanol and 0.02% polyvinyl alcohol (PVA) as a dynamic coating to reduce analytes’ interaction with the capillary wall. The samples were injected electrokinetically (10 kV, 30s) to introduce sample cations and the applied voltage was 20 kV and on-column detection at 214 nm. Several parameters affecting the separation and sensitivity of the drug and its metabolite were studied, including reconstitution solvent, organic modifier, pH and concentration of phosphate buffer. The linear ranges of the method for the simultaneous determination of the test drugs, in plasma using amlodipine as an internal standard (IS), were over the range 5-100 ng/mL for aripiprazole and dehydroaripiprazole. The application of the proposed method for determination of aripiprazole and dehydroaripiprazole in plasma collected after oral administration of 30 mg aripiprazole (Abilify??, Otsuka) daily in one schizophrenic patient was demonstrated.
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Kuo, Chi-I., and 郭俊儀. "Developing New Optical Fiber Coherence Tomography to Simultaneous Measure the Refractive Index and the Thickness of Sample." Thesis, 2003. http://ndltd.ncl.edu.tw/handle/28329996659930334559.
Full textAbstract:
碩士國立成功大學
機械工程學系碩博士班
91
Optical coherence tomography (OCT) is an optical imaging technique that allows high-resolution cross-sectional imaging of tissue microstructure. OCT such as x-ray radiography, magnetic resonance imaging, computed tomography, and ultrasonography have allowed the noninvasive cross-sectional imaging of internal structures. Recently, there have been reports of the measurement of refractive index n and thickness t by the use of OCT combined with confocal optics. These methods need to record two parameters from stage controller to solve the t and n. In order to improve accuracy of the measurement, the highly precise scanning stage is essential. However, it is not cheap. We develop a new structure to simultaneously measure the thickness and refractive index of an optical sample without implementing highly precise scanning stages by using optical fiber techniques. The system is demonstrated by two home-made samples.
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Yen, Miao-Ju, and 顏妙如. "Simultaneous determination of doxorubicin and active metabolite doxorubicinol in plasma by capillary electrophoresis and field-amplified sample stacking." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/72984624752463309016.
Full textAbstract:
碩士高雄醫學大學
藥學研究所
97
A field-amplified sample stacking and capillary electrophoresis with UV detection (CE-UV) is described for the determination of doxorubucin and doxorubicinol in human plasma. After sample pretreatment, field-amplified sample stacking method is applied for sensitive improvement. The sample was employed with an electrokinetic injection of 10 kV for 30 sec. CE separation of doxorubicin and doxorubicinol from human plasma was performed at 250C using a background electrolyte consisting of phosphate buffer (50 mM, pH 6.5) containing 16% ethylene glycol and methanol 60%. Using metformin as an internal standard (I.S.), the linear range of the method for the determination of doxorubicin and doxorubicinol was over 20.0-100.0 ng/mL. The LOD of the doxorubibin and doxorubicinol in human plasma was 5 ng/mL(S/N=3, 10 kV, 30 sec) and 10 ng/mL (S/N=3, 10 kV, 30 sec) respectively. For optimization of the procedure, the pH and strength of phosphate buffer, the volume of ethylene glycol and methanol would be discussed. Application of the method to the determination of doxorubicin and doxorubicinol in human plasma proved to be feasible.
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Hsu, Yu-Tsai, and 許育栽. "Simultaneous determination of meperidine and normeperidine in plasma by field amplified sample injection and short-end capillary electrophoresis." Thesis, 2014. http://ndltd.ncl.edu.tw/handle/bg8r7n.
Full textAbstract:
碩士高雄醫學大學
藥學研究所碩士在職專班
102
A stacking capillary electrophoresis method, field amplified sample injection and short-end injection procedure (FASI-SEIP), was developed for the determination of meperidine (MP) and normeperidine (NMP) in human plasma. MP produces analgesia by binding opioid receptors in the central nervous system (CNS). But continuous administration may result in the accumulation of NMP, responsible for CNS toxicities. It is important to establish one assay method. In this study, the capillary was filled with background electrolyte, then a water plug was injected. The electrokinetic injection was carried out, followed by a high voltage of −20 kV for separation. When analytes passed the high field region (water plug) and enter the low field region (background electrolyte), they accumulated in the interface. Finally, the analytes was stacked and separated within 2 min. The LOD (S/N= 3) was 3 ng/mL for MP and NMP, respectively. The sensitivity was about 350 folds comparing with hydrodynamic injection mode (2 psi, 10 s). During method validation, calibration curves were linear (r≧0.99) over a range from 10-500 ng/ml for MP and NMP. As the precision and accuracy assays, the absolute values of relative standard deviation (RSD) and relative error (RE) in intraday (n=3) and interday (n=5) observations were less than 8%. This method was successfully applied to real samples. After 50 mg intramuscular administration, the maximum concentration of MP was 180.7 ± 9.8 ng/mL at 30 min, and that of NMP was 64.9 ± 3.3 ng/mL at 60 min. The half-lives are 3.3 hours for MP and 18.5 hours for NMP. It was coincident to its pharmacokinetic profile in human. This method was feasible for clinical detection of MP and NMP in human plasma.
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Wang, Hsin-Jung, and 汪欣蓉. "Simultaneous determination of phenothiazine drugs in human urine sample using dispersive liquid-liquid microextraction combined with capillary electrophoresis." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/80296469338876862297.
Full textAbstract:
碩士國立高雄師範大學
化學系
103
Dispersive liquid-liquid microextraction followed by viscosity and field-amplifed sample stacking in capillary electrophoresis was determined to be a simple, fast and sensitive analytical method for simultaneously detecting three phenothiazines (promazine, chlorpromazine, and triflupromazine) in a human urine sample. The separation buffer was composed of 40mM phosphate solution (pH 2.5) and 10% (v/v) glycerol. Because glycerol exhibits viscosity, the resolution of the samples and the effect of the stacking could be substantially improved. Under optimized conditions, enrichment factors were obtained that ranged from 1190 to 2067. The proposed method for promazine, chlorpromazine and triflupromazine provided a good linearity that ranged from 0.75 to 200 nM, with correlation coefficients (r) ranging from 0.9975 to 0.9984. The limits of detection based on a signal-to-noise ratio of 3 ranged from 0.15 to 0.22 nM. The relative standard deviations of the target analytes were below 5%. The recoveries of three phenothiazines for urine samples at spiking levels of 50 to 200 nM were 87.0%~106.8%. With the advantages of a short analysis time, high enrichment factors, and high precision and accuracy, the developed method was successfully applied to determine phenothiazine drugs in human urine samples.
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Huang, Wei-Hsuan, and 黃微瑄. "1.Simultaneous determination of theophylline and dyphylline by micellar electrokinetic chromatography and application in drug formulations2.Determination of zotepine and its metabolite norzotepine in human plasma by field-amplified sample stacking." Thesis, 2004. http://ndltd.ncl.edu.tw/handle/99767450754734298049.
Full textAbstract:
碩士高雄醫學大學
藥學研究所碩士班
92
The purpose of this work is directed to the development of accurate and sensitive methods for the methylxanthines by micellar electrokinetic chromatography and the analysis of zotepine and norzotepine in plasma coupling with field amplified sample stacking. The results are summarized as follow: 1.Simultaneous determination of theophylline and dyphylline by micellar electrokinetic chromatography and application in drug formulations A simple micellar electrokinetic chromatography is described for well resolution of theophylline, dyphylline and caffeine. The separation was performed at 25℃ using a background electrolyte consisting of 10 mM borate buffer at pH 9 and 40 mM sodium dodecyl sulfate (SDS) as running buffer. Under this condition, good separation with high efficiency and short analyses time required is achieved. Several parameters affecting the separation of the drugs were studied, including the pH and concentrations of the borate buffer and sodium dodecyl sulfate. Using caffeine as an internal standard (I.S.), the linear range of the method for the determination of theophylline and dyphylline was over 0.03-1 mM, the detection limit (S/N= 3; injection 0.3 psi, 3 s) was 0.01 and 0.02 mM, respectively. 2.Determination of zotepine and its metabolite norzotepine in human plasma by field-amplified sample stacking and capillary electrophoresis A field-amplified sample stacking and capillary electrophoresis is described for the determination of zotepine and its metabolite norzotepine in human plasma. The separation was performed at 25℃ using a background electrolyte consisting of borate buffer (20 mM, pH 8) containing 50 % ethylene glycol and methanol (5:1, v/v). Using clozapine as an internal standard (I.S.), the linear range of the method for the determination of zotepine and norzotepine was over 3.0-100.0 ng/mL (r≧0.999), the detection limit was 1 ng/mL (S/N=3, electric-driven injection 20 s) and 2 ng/mL (S/N=5, electric-driven injection 20 s), respectively. Application of the method to the determination of zotepine and norzotepine in human plasma proved to be feasible.
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hua, huang yu, and 黃宇樺. "1.1. Simultaneous determination of eight antidepressants by capillary zone electrophoresis and its application in pharmaceuticals 2.Analysis of amitriptyline and its metabolite nortriptyline in plasma by field-amplified sample stacking and capillary elec." Thesis, 2003. http://ndltd.ncl.edu.tw/handle/16913115260938694078.
Full textAbstract:
碩士高雄醫學大學
藥學研究所
91
英文摘要 This study describes the establishment of capillary electrophoretic methods for the determination of eight antidepressants in available commercial formulations and the analysis of amitriptyline and nortriptyline in plasma coupling with field-amplified sample stacking. (1) Simultaneous determination of eight antidepressants by capillary zone electrophoresis and its application in pharmaceuticals A selective CZE method was established for simultaneous determination of amitriptyline, clomipramine, trimipramine, nortriptyline, protriptyline, maprotiline, doxepin and desipramine. The untreated fused-silica capillary was used (61.2 cm, effective length 50 cm, 50 mm. I.D.) for the analysis. The background buffer is Tris (0.5 M, pH 3.50) containing chiral selectors b-cyclodextrin (1.5 mM)、hydroxypropyl-b- cyclodextrin (1.5 mM) and 13 % acetonitrile. Analysis is run at the voltage of 20 kV and a detection wavelength of 200 nm. On the method validation, the calibration curves are linear over a range of 125.0-500.0 mM (r≧0.9974). The RSD and RE are all less than 3 % for the intra- and inter-day assay. All the recoveries are greater than 95 %. The limit of detection is cis-doxepine, 4 mM； protriptyline, R- or L-trimipramine, 10 mM；trans-doxepin, nortriptyline, maprotiline, amitriptyline, clomipramine, desipramine, 5 mM (S/N=5, hydrodynamic injection 3 sec). This method was feasible for the application of commercial tablets（maprotiline, amitriptyline, clomipramine） and capsules（Doxepin）. All the analytical values fall within labeled amount of 90-110 % required by the USP XXV. (2) Analysis of amitriptyline and its metabolite nortriptyline in plasma by field-amplified sample stacking and capillary electrophoresis A field-amplified sample stacking and capillary electrophoresis method is described for the determination of amitriptyline and its metabolite nortriptyline in human plasma. The untreated fused-silica capillary was used (31.2 cm, effective length 20 cm, 50 mm. I.D.) for the analysis. The background buffer is Tris (1.4 M, pH 4.50) containing b-cyclodextrin (1.0 mM) and 50 %ethylene glycol. The separation voltage is 25 kV with a detection wavelength of 200 nm. On the method validation, the calibration curves are linear over a range of 10.0-500.0 ng/mL (r≧0.9975). The RSD and RE are all less than 5 % for the intra- and inter-day assay. The relative recoveries are greater than 99 %. The limit of detection of amitriptyline and nortriptyline is 2.0 ng/mL (6.3 nM and 6.7 nM, respectively) (S/N=5, electric-driven injection 99.9 sec). One 26-yr healthy volunteer (male, 70 kg) took 125.0 mg of amitriptyline tablets. After dosing, the blood samples were drawn at 26-, 54-, and 78-hr intervals. The plasma was separated, extracted and analyzed. The levels of amitriptyline and its metabolite, nortriptyline were determinated and met closely the calculated data from pharmacokinetics of amitriptyline. A simple and sensitive CE method was applied for therapeutic drug monitoring. Comparisons between these two methods, the LODs of amitriptyline are 5 mM and 6.3 nM, respectively. The sensitivity can be raised about thousand folds by field-amplified sample stacking technique.
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Yuan, Chuang Wen, and 莊文源. "Simultaneous Dual-Capillary Column Gas Chromatographic Determination of Polychlorinated Biphenyls in Fish Samples." Thesis, 1994. http://ndltd.ncl.edu.tw/handle/83363341183649242946.
Full textAbstract:
碩士淡江大學
水資源及環境工程所
82
The lack of confirmation of identified analytes in envir- onmental gas chromatography that uses the traditional one- column , one-detector system often raises questions as to the validity of the data . To avoid misidentification of polychlorinated biphenyls ( PCB ) , we conducted simultane- ous dual-column , three detectors GC analysis . Within one GC instrument , injected sample extracts were split in two and each portion passed through a capillary column of diff- erent polarity . An electron capture detector was attached to a traditional nonpolar column , DB-5 ( 30mX0.25mm id ) for initial identification of analytes ; a more polar colu- mn , DB-17 ( 30mX0.25mm id ) , was used with the photoioni- zation detector and connected the halogen-specific electro- lytic conductivity detector with 20cm X 0.25mm id uncoated fused silica column for confirmation analysis . The separation of polychlorinated biphenyls from fish sa- mples prior to saponification of fish with sodium hytroxide -alcohol to form water-soluble products , then extracted by liquid-liquid extraction with n-hexane and K-D concentrati- on , finally used silica-gel clean-up the extracts . This configuration allows simultaneous injection of a sa- mple on two columns . The result is a more efficient , rel- iable way to identify and quantify these substances in fish samples .
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ZHANG, GUO-DA, and 張國大. "Simultaneous multielement determination of trace elements in biological samples by neutron activation analysis." Thesis, 1987. http://ndltd.ncl.edu.tw/handle/22795283974905403370.
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Wiesenfarth, Manuel. "Estimation and Inference in Special Nonparametric Models with Applications to Topics in Development Economics." Doctoral thesis, 2012. http://hdl.handle.net/11858/00-1735-0000-000D-F09E-B.
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Bojechko, Casey. "Simultaneous Analysis of Near and Far Detector Samples of the T2K Experiment to Measure Muon Neutrino Disappearance." Thesis, 2013. http://hdl.handle.net/1828/4711.
Full textAbstract:
The Tokai-to-Kamioka (T2K) experiment is a long-baseline neutrino-oscillation experiment that searches for neutrino oscillations with measurements of an off-axis, high purity, muon neutrino beam. The neutrinos are detected 295 km from production by the Super Kamiokande detector. A near detector 280 m from the production target measures the unoscillated beam. This thesis outlines an analysis using samples in the near detector and Super Kamiokande to measure the disappearance of muon neutrinos. To manage the complexity this analysis, a Markov Chain Monte Carlo framework was used to maximize a likelihood to estimate the oscillation parameters. T2K Run 1+2+3 data (3.010 x10²⁰ POT) is used for the analysis. The estimates for the oscillation parameters are:
( sin² (2θ₂₃ ), Δ m²₃₂ ) = (0.999,2.45 x10ˉ³ [eV²]),
and the 90% 1D bayesian credible intervals:
0.9340 < sin² (2θ₂₃ ) < 1.000
2.22 x10ˉ³ < Δm²₃₂ [eV²] < 2.74 x 10ˉ³Graduate
0798
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Wang, Ke-Deng, and 王科登. "Up and down shaker assisted dispersive liquid-liquid microextraction for simultaneous determination and derivatization of chlorophenols in water samples." Thesis, 2012. http://ndltd.ncl.edu.tw/handle/09994371692184269990.
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"Derivative spectrophotomtric and x-ray fluorescence spectrometric methods for the simultaneous determination of metals in alloys and water samples." Chinese University of Hong Kong, 1991. http://library.cuhk.edu.hk/record=b5886867.
Full textAbstract:
by Ho Sing Yiu.Thesis (M. Phil.)--Chinese University of Hong Kong, 1991.
Includes bibliographical references.
ACKNOWLEDGEMENT --- p.i
ABSTRACT --- p.ii
Chapter CHAPTER 1 --- GENERAL INTRODUCTION --- p.1
Chapter PART I --- DERIVATIVE SPECT3ROPHOTOMETRIC METHOD FOR THE SIMULTANEOUS DETERMINATION OF COPPER AND NICKEL IN ALLOYS
Chapter CHAPTER 2 --- INTRODUCTION --- p.5
Chapter CHAPTER 3 --- EXPERIMENTAL --- p.14
Chapter CHAPTER 4 --- RESULTS AND DISCUSSION --- p.18
Chapter PART II --- X-RAY FLUORESCENCE SPECTROMETRIC METHOD FOR THE SIMULTANEOUS DETERMINATION OF SEVEN METALS IN WATER SAMPLES
Chapter CHAPTER 5 --- INTRODUCTION --- p.43
Chapter CHAPTER 6 --- EXPERIMENTAL --- p.58
Chapter CHAPTER 7 --- RESULTS AND DISCUSSION --- p.65
Chapter CHAPTER 8 --- CONCLUSION --- p.99
REFERENCES --- p.101
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HSU, SHU-HUI, and 許淑惠. "Simultaneous Determination of Basic Drug Enantiomers in Human Urine and Serum Samples Using Capillary Electrophoresis Combined with Dispersive Liquid-Liquid Microextraction." Thesis, 2018. http://ndltd.ncl.edu.tw/handle/3n98ep.
Full textAbstract:
碩士國立高雄師範大學
化學系
106
This study was divided into two parts . First, rapid enantioseparation of three basic drugs (RS-Carvedilol, RS-Terbutaline, and RS-Metaproterenol ) was performed , with dimethyl-β-cyclodextrin (DM-β-CD) as the chiral selector and poly(diallyldimethylammonium chloride) (PDDAC) in the background electrolyte as buffer additive. Under optimized conditions, the separation system－which comprised 5mM DM-β-CD and 0.9 % PDDAC at pH 2.5 , with a capillary length of 35 cm, enabled three pairs of RS-Carvedilol, RS-Terbutaline, and RS-Metaproterenol and internal standard (losartan potassium) to be successfully separated in 10 min. Second, dispersive liquid－liquid microextraction was used in capillary electrophoresis. Under optimum conditions,the use of 1.00 mL of sample solution, 30 μL of dichloromethane as the extraction solvent, and 200 μL of acetonitrile as the dispersive solvent and, yielded a high enrichment factor in the range of 121－124 at an extraction time of less than 3 min. Moreover, a strong linearity was obtained from 0.09－to 10 μM (r >0.9956). In real samples, the recoveries of RS-Carvedilol from urine and serum samples were in the ranges of 74 %－123 % and 70 %－127 % , respectively.
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André, Maria Bernardes. "Development and optimization of an UPLC-MS/MS method for the simultaneous detection and quantification of 14 antihypertensive drugs in human urine samples." Dissertação, 2017. https://hdl.handle.net/10216/108657.
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Falconi, Ariane. "Simultaneous detection of germline and somatic mutations in DNA repair genes by next generation sequencing of tumor samples from metastatic prostate cancer patients." Dissertação, 2020. https://hdl.handle.net/10216/130970.
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André, Maria Bernardes. "Development and optimization of an UPLC-MS/MS method for the simultaneous detection and quantification of 14 antihypertensive drugs in human urine samples." Master's thesis, 2017. https://hdl.handle.net/10216/108657.
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Falconi, Ariane. "Simultaneous detection of germline and somatic mutations in DNA repair genes by next generation sequencing of tumor samples from metastatic prostate cancer patients." Master's thesis, 2020. https://hdl.handle.net/10216/130970.
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King, Jen-Yun, and 金仁筠. "Development of a multiplex PCR system for the simultaneous detection of bacillus cereus, salmonella spp. and type A enterotoxigenic staphylococcus aureus in food samples." Thesis, 1996. http://ndltd.ncl.edu.tw/handle/82877532801689884511.
Full textAbstract:
碩士國立中興大學
食品科學系
84
Bacillus cereus,Salmonella spp. and type A enterotoxigenic Staphylococcus aureus are common food-bornepathogenic bacteria. Conventional microbiologicalmethods for the detection of these bacteria normally take 5-7 days.Therefore,rapid methods for the detection of these bacteriaare important. In this study, we at first developed PCR todetect Salmonella spp. in feed and the intestinal content of chicken. Prior to the PCR enrichmenet step was used. The PCR primers TSII / TS5 would allow the amplification of a 375bp PCR product. The deection sensitivity was 10 CFU/ml. Although the PCR detection systems for Bacillus cereus,Salmonella spp. and type A enterotoxigenic Staphylococcus aureus have been reported. PCR system for the simultaneousdetection of these bacteria has not been reported, Since PCR method is one of the rapidest methods for the detection offood pathogens. In this report, We try to develope a multiplex PCR system for the simultaneous detection of B.cereus, Salmonella and type A enterotoxigenic S. aureus infood samples. Prior to the PCR assay, the targer cells mustbe enriched,For exanples type A enterotoxigenic Staphylococcus aureus, Salmonella and B. cereus could beenriched using media of 10% NaCl TSB, CTET and TSPB,repectively. The PCR conditions used are 94 J 20sec, 62 J 25sec, 72 J 30sec, with 40 PCR cycles. For this multipex PCRsystem, the primers used were A1 /A2, TSII / TS5 and Pf /Cr, and the primers ratio are 40 pmol: 3 pmol: 50 pmol. When target bacteria in cooked rice we are detected by method described above, the detection sensitivity was 10 CFU / g.
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CHANG, YA-TING, and 張雅庭. "Dispersive Liquid-Liquid Microextraction Combined with Polymer Stacking in Capillary Electrophoresis for the Simultaneous Determination of RS-Warfarin and Its Metabolite in Human Urine and Serum Samples." Thesis, 2018. http://ndltd.ncl.edu.tw/handle/srynr5.
Full textAbstract:
碩士國立高雄師範大學
化學系
106
Dispersive liquid–liquid microextraction followed by viscosity and polymer stacking in capillary electrophoresis was determined to be a simple and sensitive analytical method for detecting RS-Warfarin and its metabolite RS-7-OH-Warfarin in human urine and serum. The separation buffer comprised 200 mM Tris-borate (pH 8.5) and 0.5% (w/v) poly(ethylene oxide) (PEO). Because PEO exhibits viscosity and an intermolecular force interaction between PEO and analytes, the effect of the polymer tacking and detection sensitivity could be substantially improved. The enrichment factors obtained under optimized conditions ranged from 1758 to 1859. The proposed method for detecting RS-Warfarin and RS-7-OH-Warfarin provided a strong linearity that ranged from 1.5 to 600.0 nM, with correlation coefficients (r) ranging from 0.9952 to 0.9962. The detection limits based on a signal-to-noise ratio of 3 ranged from 0.33 to 0.38 nM. The relative standard deviations of the target analytes were all below 5% (n = 12). In the real sample, the recoveries of analytes for the urine sample at spiking levels of 50–200 nM and the serum sample at spiking levels of 0.05–2 μM were in the ranges of 91.9%–106.2% and 96.5%–103.5%, respectively. With the advantages of high enrichment factors and high accuracy and precision, the developed method was successfully applied to determine drugs in urine and serum.
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Yan, Qiao-Ting, and 顏巧婷. "Surfactant-assisted dispersive liquid-liquid microextraction combined with polymer stacking by capillary electrophoresis for the simultaneous determination of R,S-mirtazapine and its metabolites in human urine and serum samples." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/247gx4.
Full textAbstract:
碩士國立高雄師範大學
化學系
107
Surfactant-assisted dispersive liquid-liquid microextraction combined with on-line concentration - polymer stacking ( SA-DLLME-Polymer stacking ) in capillary electrophoresis was determined to be a simple and sensitive analytical method for detecting R,S-Mirtazapine and its metabolite R,S-Desmethyl mirtazapine, R,S-8-Hydroxy mirtazapine in human urine and serum. The electrophoretic analyses were carried out in 10 mM Phosphate buffer solution at pH 3.0 containing 0.9 % [Poly (diallyldimethylammonium chloride)] ( PDDAC ) and 20 mM Dimethyl-β-cyclodextrin.Because PDDAC exhibits viscosity, the effect of the polymer stacking and detection sensitivity could to substantially improved. The enrichment factors obtained under optimized conditions ranged from 2725 to 3879. The proposed method for detecting R,S-Mirtazapine and its metabolite provided strong linearity that ranged from 1.5 to 1500.0 nM, the limits of detection (LODs) ranged from 0.3 to 0.5 nM. In the real sample, the recovery of analytes for the urine sample at spiking levels of 1.5-150.0 nM and the serum sample at spiking levels of 5.0 – 250.0 nM were in the ranges of 89.0 – 116.5 % and 88.5 – 112.8 %, respectively. With the advantages of high enrichment factors and high accuracy and precision, the developed method was successfully applied to determine drugs in urine and serum.
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Wu, Chia-yen, and 吳佳燕. "1.Simultaneous Quantification of Etheno Adducts in human urine and DNA samples by Stable Isotope Dilution Capillary Liquid Chromatography/Nanospray Ionization-Tandem Mass Spectrometry 2.Post-translational modifications on human hemoglobin by glyoxal and." Thesis, 2008. http://ndltd.ncl.edu.tw/handle/39716950631837908475.
Full textAbstract:
碩士國立中正大學
化學所
96
Etheno DNA adducts are promutagenic DNA lesions derived from exogenous as well as endogenous sources. The levels of etheno adducts in tissue DNA are elevated in cancer-prone tissues, and the urinary excretion of etheno adducts is associated with oxidative stress. In this report, we have developed an assay for the accurate quantification of etheno DNA adducts by isotope dilution capillary liquid chromatography/nanospray ionization-tandem mass spectrometry (capillary LC-NSI/MS/MS) in human urine and tissue samples. These promutagenic etheno DNA adducts are excised by base excision repair and possibly the nucleotide excision repair mechanisms and they are excreted into urine as adducted bases and the nucleosides. The etheno DNA adducts investigated in this study include 1,N6-ethenoadenosine(eAde),3,N4-ethenocytidine(eCyt),1,N6-etheno-2?-deoxyadenosine(edAdo),3,N4-etheno-2?-deoxycytosine(edCyt),and1,N2-etheno-2?-deoxyguanosine(edGuo). Sample purification before analysis by MS only requires a reversed phase solid phase extraction column. The detection limit (LOD) of eAde, eCyt, edAdo, edCyt and edGuo injected on-column using this capillary LC-NSI/MS/MS is 300 , 120, 1.8, 20, and 86 amol, respectively. Levels of eAde, eCyt and edAdo in 12 human urine are 88 ± 48,109 ± 96 and 4.4 ± 3.0 pg/mL. The origin of DNA are calf thymus, human placental and human white blood cell DNA. Levels of these etheno adducts in calf thymus DNA and human placental DNA were compared as nucleosides using six different enzyme hydrolysis procedures. In human placental DNA, the levels of edAdo, edCyd and edGuo was 6.45 ± 0.46, 27.8 ± 0.27 and 7.76 ± 0.64 adducts per 107 parent nucleoside, respectively. But in some calf thymus and WBC DNA samples, the adduct levels were below the detection limits. Larger quantities of DNA is needed for simultaneous quantification of low levels of these three etheno adducts. The non-enzymatic conjugated addition product of glucose or aldehyde derivatives and glycation reaction of protein are the main cause of vascular complications of diabetes. When the concentration of glucose remains at high level in the body, the amounts of ?dicarbonyl compounds, such as glyoxal and methylglyoxal, also increase. Glyoxal is derived from glucose and amino acid oxidation as well as lipid peroxidation; whereas methylglyoxal is mainly from self-decomposition of glyceraldehyde-3-phospate (G-3-P), a degradation intermediate product. This research makes use of liquid chromatography nanospray ionization tandem mass spectrometry to investigate sites of reaction sites on human hemoglobin with glyoxal and methylglyoxal. We found that there was a single glyoxal addition at Lys-11, Lys-139, Arg-92, His-20, His-45, His-50 on ?globin and at Lys-144, His-77, His-92, His-143, Cys-93 and Cys-112 on β-globin, when the concentration of glyoxal was 20 mM. When 0.5 mM of glyoxal and methylglyoxal react with hemoglobin under physiological conditions (pH7.4, 37℃) for 48 hr, we also found that there was a single glyoxal addition at Lys-11, His-20, His-45, His-50, Arg-92 and Lys-139 on ?globin and at His-77, His-92, Cys-93, Cys-112, His-143 and Lys-144 on β-globin. For methylglyoxal, a sigle addition was found at His-20 and Arg-92 on ?globin and at Cys-93, Lys-144 on β-globin. We have also confirmed that glyoxal and methylglyoxal form hydroimidazolone at Arg-92 of ?globin. Finally, we used 0.5 μM of glyoxal and methylglyoxal to react with hemoglobin under physiological conditions (pH7.4, 37℃) for 35 days, we also found a single glyoxal addition at Lys-11, His-20, His-45, His-50 on ?globin and at His-77, His-143, His-116, Cys-93 and Cys112on β-globin. For methylglyoxal addation, only addition product of Cys-93 on β-globin was found. In human blood hemoglobin, only glyoxal addation on β-globin was found.