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1
Santos, Fabiana Almeida dos. "Adutos de DNA relacionados ao estresse oxidativo e glicação avançada em ratos diabéticos." Universidade de São Paulo, 2014. http://www.teses.usp.br/teses/disponiveis/9/9141/tde-17122014-144700/.
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O diabetes mellitus é considerado um dos problemas de saúde globalmente mais desafiadores do século 21. De acordo com as estimativas recentes do International Diabetes Federation - IDF, cerca de 382 milhões de pessoas são diabéticas e esse número tende a aumentar para além de 592 milhões em menos de 25 anos. Para melhor compreensão do Diabetes mellitus e suas complicações torna-se necessário buscar novos marcadores para a doença. O DM promove estresse oxidativo, inflamação e a formação de produtos avançados de glicação não enzimática (AGES), o que leva a dano tecidual no paciente diabético. Marcadores de dano oxidativo em proteínas e lipídeos na vigência do DM têm sido amplamente abordados na literatura, no entanto o estudo de lesões em DNA ainda requer mais atenção em modelos in vivo. Este trabalho teve como objetivo avaliar o dano oxidativo e resultante de glicação avançada em rim, fígado, cerebelo, sangue e urina de animais diabéticos, assim como a modulação do dano por diferentes períodos de tratamento com insulina, a fim de verificar se o controle da glicemia nos animais diabéticos protege contra a indução dos danos em biomoléculas. Para a indução do DM nos ratos Sprague-Dawley foram administrados 40 mg de STZ por kg de peso corpóreo por via intravenosa. Os níveis de MDA e 5-metildC foram avaliados por HPLC-DAD. A quantificação de HbA1c e dos adutos 1,N2-εdGuo, 1,N6-εdAdo, 8-oxodG e CEdG foi realizada por sistema HPLC-ESI-MS/MS. Os níveis de nitrito sérico foram determinados por leitura da absorbância em espectrofotômetro e a concentração de creatinina plasmática foi determinada por analisador bioquímico. Os resultados mostraram que as alterações metabólicas desencadeadas pela condição de hiperglicemia persistente não são prontamente revertidas após o controle da glicemia. Os níveis glicêmicos e de HbA1c apresentam diferença significativa entre os grupos de animais hiperglicêmicos e sadios, sendo observada uma queda dos valores de HbA1c somente a partir do tratamento com insulina por 6 semanas. Em plasma, rim e fígado as concentrações de MDA seguem o perfil de concentração de hemoglobina glicada (HbA1c), indicando que os eventos de glicação e estresse oxidativo podem estar relacionados. O controle glicêmico também apresentou efeito benéfico para a excreção de CEdG e 1,N6-εdAdo em urina, apesar de ser observado a partir dos níveis de 8- oxodG que a hiperinsulinemia leva a um quadro de estresse oxidativo. As três lesões são geradas por vias distintas: glicação avançada, peroxidação lipídica e ROS. Portanto, além do controle glicêmico, é importante que se desenvolvam estratégias de intervenção nas vias bioquímicas alteradas pela condição de hiperglicemia, a fim de reduzir os riscos das complicações decorrentes do diabetes mellitus.<br>Diabetes mellitus is generally considered one of the most challenging health problems of the 21st century. According to recent estimates from the International Diabetes Federation - IDF, about 382 million people have diabetes and this number is expected to increase beyond 592 million in less than 25 years. For a better understanding of diabetes mellitus and its complications becomes necessary to search for new biomarkers for the disease. The DM promotes oxidative stress, inflammation and the formation of advanced glycation end products (AGEs), which leads to tissue damage in the diabetic patient. Markers of oxidative damage to proteins and lipids in the presence of DM have been widely discussed in literature, however the study of DNA lesions in vivo models still requires more attention. This study aimed to evaluate the oxidative damage and advanced glycation in the kidney, liver, cerebellum, blood and urine of diabetic animals, as well as damage modulation for different periods of insulin treatment in order to verify that the glycaemic control in diabetic animals protects against induction of biomolecules damage. For induction of diabetes in Sprague-Dawley rats were administered 40 mg STZ per kg body weight intravenously. MDA and 5-metildC were evaluated by HPLC-DAD. The quantification of HbA1c and adducts 1,N2-εdGuo, 1,N6-εdAdo, 8-oxodG and CEdG was performed by HPLC-ESI-MS / MS system. The serum nitrite was determined by reading the absorbance in a spectrophotometer and the plasma creatinine concentration was determined by biochemical analyzer. The results showed that metabolic changes triggered by the condition of persistent hyperglycemia are not readily reversed after glycemic control. Blood glucose and HbA1c levels are significantly different between the groups of hyperglycemic and healthy animals, and was observed a fall in HbA1c only from insulin treatment for 6 weeks. In plasma, kidney and liver concentrations follow the profile of MDA concentration of glycated hemoglobin (HbA1c), indicating that the events of glycation and oxidative stress may be related. Glycemic control also showed beneficial effect for urine excretion of CEdG and 1,N6-εdAdo despite could be seen from 8-oxodG levels that the hyperinsulinaemia leads to a frame of oxidative stress. The three lesions are generated by distinct pathways: advanced glycation, lipid peroxidation and ROS. Therefore, beyond glycaemic control, it is important to develop intervention strategies in biochemical pathways altered by the condition of hyperglycemia in order to reduce the complications risk of diabetes mellitus.
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Aljohani, Wael Hamad H. "Fabrication and characterisation of organic monolithic columns for the separation of small molecules using HPLC-MS : the Frame Problem revisited." Thesis, King's College London (University of London), 2017. https://kclpure.kcl.ac.uk/portal/en/theses/fabrication-and-characterisation-of-organic-monolithic-columns-for-the-separation-of-small-molecules-using-hplcms(b5ace486-6de8-4a35-ba45-6024e6bea2b7).html.
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Monolithic columns are continuous interconnected networks with large through-pore channels. This structure results in a decrease in the diffusion path and affords high permeability, which result in obtaining good separation efficiency. Ideally, the structure of monoliths should be bi-model consisting of meso-pores and macro-pores responsible for retention time and flow of mobile phase respectively. The structure also enhances the mechanical strength, and the large through-pore channels afford very low flow resistance. This combination therefore results in the ability of smaller diameter monolithic columns to be employed under high flow rates, increasing both sensitivity and throughput simultaneously. Additionally, the unique structure of monoliths improves permeability and mass transfer leading to a decrease in band broadening. The first stage of the project was focused on the fabrication and characterisation of an organic monolithic column namely poly (SMA-co-EDMA) followed by quantification of caffeine in Arabic coffee. Since the efficiency of the above monolith was low due to the low number of mesopores (low surface area), the second stage was centered on improving the efficiency of organic monoliths via the use of a longer crosslinker namely 1,6-HEDA. This novel monolith column poly (HMA-co-1,6-HEDA) afforded high efficiency, good porosity, high permeability and excellent reproducibility. Next, this monolith was applied to several applications namely separation of neutral non-polar analytes, weak acids, and strong bases, followed by a quantification of amitriptyline in commercial pharmaceutical tablets. Since the results obtained for this novel monolith using capillary liquid chromatography were encouraging, the third stage was investigating the possibilities of coupling narrow fused silica capillaries with mass spectrometry (MS). In this stage, the novel monolith (HMA-co-1,6- HEDA) lacked stability under high pressure due to either the low concentration of the crosslinker (1,6-HEDA) in the polymerisation mixture or the ratio between the monomer mixture (HMA and 1,6-HEDA) and porogen system (1-propanol and 1,4-butanediol). Hence, a move towards using nano-flow to couple narrow fused silica capillaries to the MS was utilised and was successful in separating two basic drugs (amitriptyline and nortriptyline). Finally, in order to widen the application of reversed- phase monoliths, a new monolithic material namely poly (GMA-co-EDMA) was synthesised followed by incorporation of high purity Congo red (CR) which contains several functional groups including SO3H, and then evaluating by separation of some reversed phase and HILIC mixtures.
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Bakirdere, Sezgin. "Speciation Studies Using Hplc-icp-ms And Hplc-es-ms." Phd thesis, METU, 2009. http://etd.lib.metu.edu.tr/upload/3/12611391/index.pdf.
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Knowledge about selenium content of foods containing selenium species is very important in terms of both nutrition and toxicity. Bioavailability of selenium species for human body is different from each other. Hence, speciation of selenium is more important than total selenium determination. In the selenium speciation study, chicken breast samples, selenium supplement tablets and egg samples were analyzed for their selenium contents. In chicken breast study, chickens were randomly categorized into three groups including the control group (25 chickens), inorganic selenium fed group (25 chickens) and organic selenium fed group (25 chickens). After the optimization of all the analytical parameters used throughout the study, selenomethionine, selenocystine, Se(IV) and Se(VI) were determined using Cation Exchange-HPLC-ICP-MS system. In selenium supplement tablet study, anion and cation exchange chromatographies were used to determine selenium species.
Arsenic is known as toxic element, and toxicity of inorganic arsenic species, As(III) and As(V), is much higher than organic arsenic species like arsenobetaine and arsenosugars. Hence, speciation of arsenic species in any matrix related with human health is very important. In the arsenic speciation study, Cation Exchange-HPLC-ICP-MS and Cation Exchange-HPLC-ES-MS systems were used to determine arsenobetaine content of DORM-2, DORM-3 and DOLT-4 as CRMs. All of the parameters in extraction, separation and detection steps were optimized. Standard addition method was applied to samples to eliminate or minimize the matrix interference.
Thiols play an important role in metabolism and cellular homeostasis. Hence, determination of thiol compounds in biological matrices has been of interest by scientists. In the thiol study, Reverse Phase-HPLC-ICP-MS and Reverse Phase-HPLC-ES-MS systems were used for the separation and detection of thiols. For the thiol determination, thiols containing &ndash<br>S-S- bond were reduced using dithiothreitol (DTT). Reduction efficiencies for species of interest were found to be around 100%. Reduced and free thiols were derivatized before introduction on the column by p-hydroxymercuribenzoate (PHMB) and then separated from each other by using a C8 column. In the real sample measurement, yeast samples were analyzed using HPLC-ES-MS system.
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Forss, Erik. "On-line HPLC." Thesis, Karlstads universitet, Avdelningen för kemiteknik, 2012. http://urn.kb.se/resolve?urn=urn:nbn:se:kau:diva-16166.
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In order to increase the analysis frequency and thereby achieve a better understanding of the kinetics and dynamics of the chemical process without increasing the workload of the already strained analytical laboratory at Cambrex Karlskoga AB, this projects goal was to investigate whether a crude prototype for mobile on-line HPLC-analysis with automatic sampling and dilution could be built based on certain flow-injection analysis techniques. It was possible to achieve dilution with good repeatability even though saturation effects in the filter proved problematic. Separation and dilution of a binary mixture was also successful as proof-ofconcept.
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Kadkhodaei-Elyaderani, Manizheh. "HPLC detection of haemoglobinopaties." Thesis, University of Salford, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.308175.
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Ertas, Hasan. "Ageing of silica in HPLC." Thesis, Loughborough University, 1998. https://dspace.lboro.ac.uk/2134/33118.
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This study may be divided into two sections which cover different aspects of the reproducibility problems encountered in HPLC. In the first, the study has involved the separation of basic drugs, on different manufacturer's reversed-phase columns in conjunction with an acid buffered acetonitrile/water gradient. The retention reproducibility of each drug was assessed and compared on the basis of the retention index scale of 1-nitroalkanes. The effect of changing gradient run time on the reproducibility of the retention values of the 1-nitroalkanes was demonstrated on reversed-phases of different makers. The optimisation of initial isocratic composition of organic (acetonitrile) was carried out and its effect on the reproducibility of retention of basic drugs was evaluated. The effect of a premixed eluent on the retention reproducibility of selected basic drugs with time intervals between injections was demonstrated. The same method was further extended with or without using helium gas with small flow. The prediction of dwell volume and its effect on retention reproducibility was evaluated. Determination of retention times changes for selected aqueous basic solutes against eluent with different pH values on Capcell ODS column was studied. Applicability of each reversed-phases (Cl8) for the separation of basic analytes was demonstrated. In the second section, a number of different unbonded (bare) silicas were studied in terms of surface analysis using of solid state cross-polarisation (CP) magic angle spinning (MAS) NMR and Fourier Transform (FT) Diffuse Reflectance Infrared Spectra (DRIFT-IR) data. It is believed that silica material used for HPLC separation with eluent undergoes an ageing process with acidic (at pH:2–3) and basic eluents (higher than pH:8). To examine this process more clearly, some basic analytes were selected to evaluate each of the accelerated ageing process followed by showing the final surface properties by the method most commonly used such as solid-state NMR and FT-IR along with BET surface analyser.
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Burr, Christina Mary. "Retention prediction in RP-HPLC." Thesis, Loughborough University, 1988. https://dspace.lboro.ac.uk/2134/27346.
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A method of calculating the RP-HPLC retention indices, based on the alkylarylketone scale, has been developed. The retention indices are calculated from the molecular structure of a compound as the sum of the parent contribution, the parent index, the substituent contributions, the substituent indices, and terms to account for the interactions between substituents, the interaction indices.
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Mayr, Gerhard. "Bildung und Kompensation von Temperaturgradienten in der schnellen HPLC unter Verwendung von Micropartikel-gepackten HPLC-Säulen." Ulm : Universität Ulm, Fakultät für Naturwissenschaften, 1999. http://www.bsz-bw.de/cgi-bin/xvms.cgi?SWB8303640.
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Müller, Sonja. "Analytische Trennungen neuartiger Supramoleküle mittels HPLC." [S.l.] : [s.n.], 2006. http://deposit.ddb.de/cgi-bin/dokserv?idn=980196973.
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Thomas, H. D. "Chemiluminescence, a detection method for HPLC." Thesis, University of East Anglia, 1988. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.383774.
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Scholtzova, Angela. "Scale up and modelling of HPLC." Thesis, University College London (University of London), 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.368109.
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Albishri, Hassan Mabrook. "High-temperature HPLC of pharmaceutical compounds." Thesis, Loughborough University, 2007. https://dspace.lboro.ac.uk/2134/36130.
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In this thesis, we established methods that use high-temperature HPLC for the efficient separation of different groups of pharmaceutical compounds. These groups are cephalosporins, non-steroidal anti-inflammatory (NSAID), and diuretic drugs. The effect of changes of the temperature of the column was studied with respect to various chromatographic parameters: retention factors, thermodynamic properties, selectivity, efficiency and peak shape. Three columns (Pathfinder, Xterra RP18, and Selerity's Blaze 200) were examined for the analysis of cephalosporin drugs under high temperature reversed phase HPLC. Several proportions of mobile phases were used with these columns. This study focused on the effect of column temperature on selectivity (α), and efficiency (N/m), van't Hoff plots. The best conditions for the separation of these drugs were 60 °C with 100% water as eluent and these conditions were the best for quantitative applications. This condition was validated according to International Conference on Harmonisation (ICR) with respects of linearity, limit of detection (LOD), limit of quantification (LOQ), and precision (tR, relative peak area %, N/m).
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Madahar, Kirpal C. "The determination of ethylenethiourea by HPLC." Thesis, Loughborough University, 1986. https://dspace.lboro.ac.uk/2134/32913.
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The determination of imidazolidine-2-thione (ETU), at residue levels in crops, in ethylenebisdithiocarbamates (EBDC) and on interaction with microorganisms and soils has been investigated using both a direct HPLC method or after derivatisation with phenacyl halides.
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Che, Isa Rosmahani. "Analysis of rubber accelerators by HPLC." Thesis, Loughborough University, 2009. https://dspace.lboro.ac.uk/2134/34256.
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The analysis of rubber accelerators particularly zinc dithiocarbamates (ZDTCs) was carried out by high performance liquid chromatography (HPLC) to develop an improved analytical method for the determination of rubber accelerators. Further understanding of their chemical and chromatographic behaviour has been established by investigating a few conventional as well as the latest reported methods, which include the pre-column derivatisation of ZDTCs to cobalt (III) complexes, direct determination by the addition of other protective agent and pre-column derivatisation of ZDTCs to copper (III) complexes.
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Walker, Roderick Bryan. "HPLC analysis and pharmacokinetics of cyclizine." Thesis, Rhodes University, 1995. http://hdl.handle.net/10962/d1003279.
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The investigations detailed in this dissertation have been conducted to address the paucity of pharmacokinetic information, in published literature, pertaining to cyclizine. The areas of investigation have included the selective quantitation of both cyclizine and its demethylated metabolite, norcyclizine in serum and urine, assessment of stability of both compounds in stored biological samples, dosage form analysis, dissolution rate testing of tablets, and bioavailability and pharmacokinetics following administration of an intravenous solution, and tablets to humans. High-performance liquid chromatography (HPLC) was used as the main analytical technique throughout these studies. An original HPLC method employing ultraviolet detection with a limit of quantitation of 5μg/ℓ was developed for the determination of cyclizine in serum and both cyclizine and norcyclizine in urine, Solid-phase extraction using extraction columns packed with reversed-phase C18 material, and followed by a simple phase-separation step proved successful for the accurate and precise isolation of the compounds. The validated method was applied to the analysis of serum and urine samples from a pilot study in which a single volunteer was administered 50mg of cyclizine hydrochloride. Several samples collected during the pilot study revealed the presence of both drug and metabolite in concentrations below the limit of detection. In order to improve the selectivity and sensitivity of the analytical method an HPLC method with electrochemical detection operating in the "oxidative-screen" mode was developed. The solid-phase extraction procedure was modified slightly and the method found to be precise, accurate, selective and highly sensitive with a limit of quantitation of Iμg/g/l for both cyclizine and norcyclizine in both serum and urine. This method was applied to the determination of both compounds after intravenous and oral administration of cyclizine to humans. HPLC with electrochemical detection was used for the analysis of samples collected during dissolution studies on the batch of tablets used for pharmacokinetic studies. In addition, this method was used to assess content uniformity of the tablets and of samples from the batch of intravenous ampoules of cyclizine lactate. Dissolution studies showed that all tablets tested passed the compendial specifications for cyclizine. Content uniformity assessment revealed that within-batch uniformity existed for both the tablets and ampoules and, therefore, variations in pharmacokinetic parameters for the drug would more than likely be as a result of inter- and intra-individual variability within the subject population. Pharmacokinetic information for cyclizine was obtained following administration of an intravenous bolus dose of cyclizine lactate as a solution, oral administration of cyclizine hydrochloride as a single dose of 50mg and as fixed multiple doses of 50mg every 8 hours for five days. Further information was acquired following administration of single doses of 100mg and 150mg cyclizine hydrochloride. Data collected from these studies were evaluated using both compartmental and non-compartmental techniques. Cyclizine was rapidly absorbed following oral administration with mean kₐ = 1.54 hr⁻¹ and was found to have an absolute bioavailability (F) of 0.47. The presence of norcyclizine in serum following oral and not intravenous dosing suggests cyclizine is susceptible to "first-pass" metabolism in either the gut wall or the I iver. Mean ClTOT determined following the intravenous dose was 0.865 ℓ/hr/kg. The mean ClTOT of 0.823 ℓ/hr/kg calculated following oral dosing, using a unique value of F for each subject compared favourahly with that obtained following intravenous dosing. Renal clearance of cyclizine is negligihle indicating that non-renal routes of elimination account for the majority of removal of cyclizine form the body. Cyclizine is extensively distributed and the mean Vz following an intravenous dose was 16.70 ℓ/kg. This value is lower than that calculated from all oral studies from which the mean Vz was determined to be 25.74 ℓ/kg. Cyclizine is eliminated slowly with a mean elimination t½ = 20.11 hours. Cyclizine dose not appear to follow dosedependent kinetics and therefore, inability to predict steady state levels are more than likely due to accumulation as a result of frequent dosing rather than saturation of elimination mechanisms. Modelling of intravenous data to one-compartment (lBCM), two-compartment (2BCM) and threecompartment models indicated that the pharmacokinetics of cyclizine can be adequately described by a 3BCM. The drug is rapidly distributed into a "shallow" peripheral compartment (α = 9.44 hr⁻¹ , and k₂₁ = 2.09 hr⁻¹ ), and slowly distributed to the "deep" peripheral compartment (β = 0.451 hr⁻¹ and k₃₁ = 0.120 hr⁻¹ ). Modelling of all oral data indicated that a 2BCM best described the pharmacokinetics of the drug, however, distribution to the peripheral compartment is not as rapid as to the "shallow" peripheral compartment following the intravenous dose. Mean distribution parameters were α = 0.64 hr⁻¹1 and, k₂₁ = 0.39 hr⁻¹. Mean CITOT following intravenous dosing of 0.70 ℓ/hr/kg was similar to the mean CIToT of 0.73 ℓ/hr/kg determined after oral dosing. The mean distribution volume at steady state determined following intravenous dosing (17.78 ℓ/kg) was lower than that obtained from the oral studies (25.52 ℓ/kg). The mean terminal elimination half-lives calculated for cyclizine following fitting of intravenous and oral data was 25.09 hours. In general, mean pharmacokinetic parameters calculated following titting of data to a 2BCM after oral administration correlate closely with those calculated using non-compartmental techniques. However, the pharmacokinetics following intravenous dosing are better described by a 3BCM and a close correlation between parameters estimated using noncompartmental techniques and compartmental techniques is evident when a 3BCM model is used.
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Mayr, Gerhard [Verfasser]. "Bildung und Kompensation von Temperaturgradienten in der schnellen HPLC unter Verwendung von Micropartikel-gepackten HPLC-Säulen / Gerhard Mayr." Ulm : Universität Ulm. Fakultät für Naturwissenschaften, 1999. http://d-nb.info/1015899285/34.
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McCulloch, Melissa. "Development of Quantitative Bioanalytical Methods for the Measurement of Pharmaceutical Compounds via HPLC-UV and HPLC-MS/MS." Cleveland State University / OhioLINK, 2009. http://rave.ohiolink.edu/etdc/view?acc_num=csu1255046678.
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Westlake, James P. "The analysis of basic drugs by HPLC." Thesis, Loughborough University, 1991. https://dspace.lboro.ac.uk/2134/10517.
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Two methods for the high performance liquid chromatographic analysis of basic drugs have been studied. In each case the methods have concentrated on separating drugs of forensic interest, based on specially designed test solutions of analytes selected to represent most of the commonly encountered classes of drug compounds. In the first case, a HPLC method was developed on unmodified silica using an aqueous methanolic eluent of high pH. The buffer was prepared from two organic sulphonic acid amines, 3-(cyclohexylamino)-1- propanesulphonic acid (CAPS) and sodium 3-(cyclohexylamino)-2-hydroxy-1- propanesulphonate (CAPSO-Na). The method was shown to be highly reproducible within a single laboratory. The long term stability of the unmodified silica stationary phase was examined, using the newly developed method for the analysis of drugs as a monitor of column performance. Three columns from a single batch of silica were studied, and all showed pronounced changes in retention properties over the period of the study. Similar changes in retention properties were observed for silica stored dry and unused. These results led to the idea that an 'aging process' was changing the nature of the silica surface, probably by a process of hydrolysis of surface siloxanes. This aging process was also believed to be responsible for the appearance of distorted peak shapes for methylamphetamine, although no clearly defined mechanisms could be found to support this idea. In a second study, the application of gradient HPLC methods for the screening ·of a wide range of analytes was examined. In this case, an Inertsil ODS-2 column was used in conjunction with an acid buffered acetonitrile I water gradient. The usefulness of the 1-nitroalkanes as a retention index series was demonstrated and a good level of retention reproducibility was achieved for most analytes studied.
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Tebrake, Margret G. "Temperature as a parameter in HPLC optimisation." Thesis, Loughborough University, 2003. https://dspace.lboro.ac.uk/2134/33879.
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This study focused on the capabilities of elevated temperature chromatography and its potential applications. The effects of separation temperature on compound retention, selectivity and efficiency were studied. The change in retention with temperature was explored using a number of test compound solutions. A detailed investigation of the importance of system variables like dead volume, mobile phase composition, different stationary phases, and temperature control of column and eluent was performed. The effects of different eluents and different means of temperature control on the separation selectivity and efficiency were investigated and results were compared.
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Zahr, Meia. "Separation of Tryptic Digested IgG with HPLC." Thesis, KTH, Skolan för kemi, bioteknologi och hälsa (CBH), 2018. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-233869.
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The antibody immunoglobulin G (IgG) can be tryptically digested into smaller peptides. This study attempted to develop a separation method for those peptides using RP-HPLC with a C18 column at room temperature. Optimizing separation of trypsin cleaved cytochrome C was used as a guideline before analyzing IgG. The optimized analysis of Cytochrome C was performed at wavelength 280nm (UV) and methanol was used as an organic solvent in mobile phase (B). A fast gradient to 100% mobile phase B with low flow rate gave favorable results for cytochrome C. A slow gradient to 100% mobile phase B was suited for IgG separation. The optimized gradient elution of cytochrome C and IgG was performed at 0.3 and 0.8 ml/min, respectively.<br>Antikroppen Immunoglobulin G (IgG) kan klyvas till peptider med enzymet trypsin. Under denna studie ska utvecklades en separationsmetod för dessa peptider med RP-HPLC. Separationen utfördes med en C18 kolonn i rumstemperatur. Först optimerades en separation av trypsin-klyvt cytokrom C vars optimerade parametrar sedan användes som grund för IgG-separation. Optimeringen utfördes vid våglängden 280 nm(UV) och metanol användes som organiskt lösningsmedel i mobil fas (B). En snabb gradient upp till 100% B med låg flödeshastighet gav mest gynnsamt resultat för cytokrom C. Separationen av IgG gynnades av ett högt flöde och en långsam gradient till 100% B. Den optimerade gradientelueringen för cytokrom C och IgG gjordes vid flödet 0.3 respektive 0.8 ml/min.
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Käsmä, S. (Salla). "(U)HPLC-MS/MS käyttö virtsanäytteiden steroidianalyyseissä." Bachelor's thesis, University of Oulu, 2019. http://urn.fi/URN:NBN:fi:oulu-201901121055.
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Kehossa esiintyy luontaisesti useita anabolisia androgeenisia steroidiyhdisteitä, joista lihasmassan kasvun ja sen ylläpidon kannalta merkittävin on testosteroni. Testosteronin voimakkaan anabolisen vaikutuksen takia siitä on tehty useita muunnelma, joilla on pyritty minimoimaan androgeenista vaikutusta, maksimoimaan anabolista tehoa ja esimerkiksi vaikuttamaan yhdisteen vapautumiseen kehossa. Luontaisetja synteettiset anaboliset androgeenit ovat sekä rakenteeltaan että toiminnaltaan testosteronin kaltaisia. Anabolisten androgeenien ja muiden steroidiyhdisteiden aineenvaihdunta on monimutkaista, sisältäen useita entsyymiavusteisia reaktioita, minkä johdosta steroidiyhdisteiden analysointi voi olla haastavaa ja tiettyä yhdistettä voidaan tutkia suoraan tai useiden eri markkerien tai metaboliittien avulla.
Steroidiyhdisteiden analytiikassa aineenvaihdunta huomioidaan näytteenkäsittelyssä. Virtsan sisältämät steroidit ovat suurilta osin glukuronidikonjugaatteja, joiden lisäksi virtsassa esiintyy sulfaattikonjugaatteja ja muita aineenvaihduntatuotteita. Näytteenkäsittelyssä glukuronidikonjugaatit yleensä hydrolysoidaan takaisin vapaaseen steroidimuotoon ja näytteet uutetaan poolittomien ja poolisten yhdisteiden erottamiseksi. Laitekomponenttien ja menetelmän kehittyminen on mahdollistanut myös suoraruiskutusmenetelmän soveltamisen.
Steroideja voidaan analysoida virtsasta perinteisen kaasukromatografia-massaspektrometrin lisäksi mm. korkean erotuskyvyn nestekromatografialla kytkettynä tandem massaspektrometriin. Menetelmää voidaan käyttää sekä kvantitatiivisiin että kvalitatiivisiin analyyseihin ja sen etu on lämpöherkkien yhdisteiden analysointi, herkkyys ja automaation helppous. Steroidianalyyseissä nestekromatografisessa erotuksessa käytetään yleisimmin käänteisfaasierotusta ja gradienttimenetelmää. Ionisointi suoritetaan sähkösumutusionisaatiolla tai kemiallisella ionisaatiolla normaali ilmanpaineessa, sillä kyseiset ionisaatiomenetelmät aiheuttavat vähän fragmentaatiota. Massa-analysaattorina käytetään yleisimmin kolmoiskvadrupolia, mutta myös ioniloukku- ja lentoaika-analysaattoreita yhdistettynä kvadrupoliin.
Korkean erotuskyvyn nestekromatografia kytkettynä tandem massaspektrometriin sisältää useita eri muuttujia, joita vaihtelemalla, säätämällä ja optimoimalla voidaan vaikuttaa analyysituloksiin. Menetelmän erilaisten mahdollisuuksien määrä mahdollistaa lukuisten erilaisten yhdisteiden analysoinnin ja menetelmän edelleen kehittymisen.
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Puč, Vojtěch. "Stanovení beta-karotenu v ječmeni metodou HPLC." Master's thesis, Vysoké učení technické v Brně. Fakulta chemická, 2008. http://www.nusl.cz/ntk/nusl-216413.
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This diploma thesis deals with the natural antioxidants present in cereals, especially in barley (Hordeum vulgare). A close attention is paid to the study of carotenoids determination was conducted. In the experimental part, the method of beta-carotene determination was optimized using high-performance liquid chromatography, diode array detector and mass detector (HPLC/DAD/APCI-MS). The method was used for the beta-carotene and lutein determination in the samples of barleycorn, malt and green barley. This method involves the sample saponification, extraction by diethylether, followed by separation on ODS Hypersil 250x4,6 mm, 5m column, using MTBE/MeOH (20:80) as mobile phase and spectrophotometric detection (450 nm). Quantitative analysis was implemented in the HPLC/DAD system. The MS detector was used for identification of analytes. A number of still unpublished data about the content of beta-carotene and lutein in several varieties of malting barley, malt and green barley are stated in this thesis. The highest content of beta-carotene was found in the green barley sample of variety Malz, harvested in first grow phase (8,49 mg/kg of the dry matter). The content of beta-carotene in barleycorn is relatively low (0,07-0,14 mg/kg of the dry matter). The content of beta-carotene is several times higher in the malt produced from barleycorn (0,24-0,56 mg/kg of the dry matter). The diploma thesis was implemented in the Research Institute of Brewing and Malting, Plc. in Brno.
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Králová, Radka. "Stanovení léčiv v pitných vodách metodou HPLC." Master's thesis, Vysoké učení technické v Brně. Fakulta chemická, 2015. http://www.nusl.cz/ntk/nusl-217167.
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The aim of the diploma thesis is the determination of macrolide antibiotics in drinking water by using of high performance liquid chromatography. Erythromycin and clarithromycin were selected such as representative macrolides due to frequently prescribed pharmaceuticals in this time. Solid phase extraction (SPE) by using of Oasis HLB cartridges was applied for pre concentration and purification of chosen analytes in real samples of drinking water. Optimalization of method and analysis were performed by using of high performance liquid chromatography with mass spectrometry detection (HPLC-MS). The suitable method was selected for determination of macrolides in real samples taken from two sources of drinking water, the interception of water in Litovel and Černovír Olomouc.
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Dohnalová, Monika. "HPLC analýza léčiv." Master's thesis, 2019. http://www.nusl.cz/ntk/nusl-397354.
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Charles University Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Monika Dohnalová Supervisor: Ing. Vladimír Kubíček, CSc. Title of Diploma Thesis: HPLC analysis of drugs The diploma thesis deals with the development and optimization of HPLC method for simultaneous determination of selected polyphenolic compounds: apigenin, acteoside and luteolin. During the experiments, the most suitable conditions for separation were sought, various mobile phases and various types of gradient elution were tested. The Zorbax Eclipse XBD C18 column 250 x 4.6 mm; 5 µm was used for analysis. The detection was performed with diode array detector at wavelengths 249 nm and 350 nm,the column was thermostated at 30 řC. The injected volume was 10 µl. The best results were achieved using mobile phase consisting of acetonitrile and aqueous solution of formic acid (0.03 mol/l) at a flow rate 1ml/min.
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Kouřil, Tomáš. "HPLC analýza léčiv." Master's thesis, 2018. http://www.nusl.cz/ntk/nusl-388725.
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Charles University Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Tomas Kouril Consultant: Ing. Vladimir Kubicek, CSc. Title of Thesis: HPLC analysis of Drugs The diploma thesis describes selection of the most suitable conditions for determination of a two enantiomers of drugs betaxolol and bisoprolol with a method HPLC. The aim of the thesis was to find a suitable isocratic method for the substances for extraction from plasma. The chromatographic column Daicel Chiralcel ® OD-R 4,6 mm x 250 m was utilized. The best results were achieved with mobile phase consisting of acetonitrile and aqueous solution of sodium perchlorate (1 molar) in volume ratio 50:50 for betaxolol and 35:65 for bisoprolol. The column was thermostated at 25 řC. UV detection (λ = 190 nm) was applied to get a sufficient sensitivity. Tramadol and O-desmethyltramadol was tested as an internal standard. Biological samples were tested by LLE before the HPLC analyses. Furthermore, the LLE method for biological samples was tested before performing HPLC.
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Nováková, Markéta. "HPLC analýza podofylotoxinu." Master's thesis, 2021. http://www.nusl.cz/ntk/nusl-446527.
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Charles University, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Pharmaceutical Analysis Candidate: Markéta Nováková Tutor: PharmDr. Pavla Pilařová, Ph.D. Title of Thesis: HPLC Analysis of Podophyllotoxin The diploma thesis is focused on optimalization of HPLC method for the analysis of podophyllotoxin. The method was developed for the analysis of Juniperus virginiana leaves extract. Various stationary phases, mobile phases, temperatures, ultrasonic extraction times were tested. Following conditions were chosen as optimal: 30 minutes ultrasonic extraction time, LiChrospher 100 RP-18 250-4 column, 0,1% CH3COOH:ACN 45:55 mobile phase, temperature 40 řC, flow rate 0,8 ml/min, sample volume 3 μl, fluorescence detection λex 240 nm, λem 320 nm, time of analysis 9 minutes. The method was also developed for the analysis of plant tissue cultures of Juniperus virginiana, for which gradient elution was chosen. This method had following conditions: LiChrospher 100 RP-18 250-4 column, mobile phase 0,1% CH3COOH:ACN, change of acetic acid ratio: 0-8 min 70-10 %, 8-9 min 10 %, 9-10 min 10- 70 %, 10-12 min 70 %, temperature 40 řC, flow rate 0,8 ml/min, sample volume 3 μl, fluorescence detection λex 240 nm, λem 320 nm, time of analysis 12 minutes. Subsequently, both methods were...
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Lukšíková, Lada. "HPLC analýza léčiv." Master's thesis, 2009. http://www.nusl.cz/ntk/nusl-282942.
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Slezáková, Šárka. "HPLC stanovení benzimidazolů." Master's thesis, 2015. http://www.nusl.cz/ntk/nusl-337823.
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Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of biophysics and physical chemistry Candidate: Šárka Slezáková Supervisor: Ing. Vladimír Kubíček, CSc. Title of diploma thesis: HPLC Determination of Benzimidazoles In this thesis we have investigated the possibility of establishing benzimidazole with HILIC chromatography using a chromatographic column Ascentis Express HILIC 10.0 cm x 3.0 mm; 2.7 microns. Two groups of benzimidazoles were tested. The first one was focused on albendazole and its metabolites. Experiments with these substances did not produce satisfactory results, because the mobile phase composition which enables separation of the studied analytes was not found. The second group was formed by flubendazole and its reduced and hydrolyzed form. In this case, several mobile phase compositions were tested. Finally, distribution of individual analytes in a mixture, using a mobile phase ACN:HCOOH 0.03 mol/l (90:10), was successfully achieved. Ricobendazol was chosen as an internal standard. When separation conditions were found, calibration curve for the determination of reduced flubendazole in biological samples was subsequently constructed using ricobendazol as the internal standard with the use of fluorescence detection. Keywords: HILIC, HPLC, albendazole,...
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Nováková, Lidmila. "HPLC analýza vybraných isoflavonů." Master's thesis, 2020. http://www.nusl.cz/ntk/nusl-435323.
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Charles University Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Author: Lidmila Nováková Supervisor: Ing. Vladimír Kubíček, CSc. Title of thesis: HPLC analysis of selected isoflavones The diploma thesis deals with the development of a method for determination of the concentration of selected isoflavones in samples of biological material by using HPLC. The method is applicable to both glycosylated (daidzeine, genistine and glycitine) and free forms of isoflavones (daidzeine, genisteine). The Ascentis® Express RP column 2,7 µm, 10 cm x 3 mm was used for analysis. The mobile phase was composed of a solution of formic acid and acetonitrile and the measurement was performed in a gradient elution mode. The constant flow rate of the mobile phase was set at 0.5 ml / min. The column was thermostated at 30 ř C. The sample injection volume was 10 µl. UV detection was performed at 249 nm and 260 nm. Six samples of biological material containing isoflavones were analyzed consequently. Based on the calibration previously carried out, concentrations of the isoflavones were determined in the biological samples. Key words: HPLC, daidzine, genistine, glycitine, analysis
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Koldová, Vendula. "Hodnocení Quetiapinu pomocí HPLC." Master's thesis, 2015. http://www.nusl.cz/ntk/nusl-334696.
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Charles University in Praque, Faculty of Pharmacy in Hradci Králové Department: Pharmaceutical Chemistry and Drug Control Candidate: Vendula Koldová Tutor: PharmDr. Pavla Pilařová, Ph.D. Name of Degree Paper: Evaluation of Quetiapine using HPLC In this study was developed a method for separation of quetiapine and its two biologically active metabolites 7-hydroxyquetiapine and norquetiapine. Separation was performed on zirconia reversed-phase column ZirChrom® -PBD (150 x 4.6 mm i.d., 5 µm). The retention behaviour of those three analytes was examined at changing strenght and pH of acetate buffer and changing levels of organic compound (ACN) in eluent. The separation of the mixture of quetiapine and its two metabolites was performed by gradient elution. Mobile phase was composed of acetate buffer (CH3COONH4 6mM , pH 6.0) and acetonitrile. The flow rate of the mobile phase was 1.0 ml/min and temperature in the column was set at 30 řC. Detection was carried out at a wavelength of 254 nm. The method is supposed to be used for determination of quetiapine, 7-hydroxyquetiapine and norquetiapine in plasma.
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Chang, Chih-Chao, and 張智超. "HPLC quantitative analysis of." Thesis, 2008. http://ndltd.ncl.edu.tw/handle/742tcg.
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Juříčková, Markéta. "HPLC analýza léčiv II." Master's thesis, 2010. http://www.nusl.cz/ntk/nusl-282921.
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HPLC ANALYSIS OF DRUGS II. Diploma thesis Markéta Juříčková Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové In diploma thesis the optimal condition for analytical determination of tiaprofenic acid in plasma using solid-phase microextraction (SPME) and high performance liquid chromatography (HPLC) was developed. The final analysis was performed on RP18 analytical column. The mobile phase was composed of a mixture of methanol and phosphate buffer. The flow rate of 0.7 ml/min was used. 20 µl of sample was injected on the column. Detection was performed in UV range at 306 nm. PDMS/DVB microextraction fiber was used for the isolation of tiaprofenic acid from the sample. At first tiaprofenic acid was isolated from the water solution. Recovery of the microextraction was 19.46 %. Thereafter, tiaprofenic acid was extracted from model plasma sample. Prior extraction, pH of plasma was adjusted on 2.8. Methanol was used for analyte desorption. Optimal time of sorption and desorption was also determined. Efficiency of the developed extraction was 9.74 %. Quantitative determination of tiaprofenic acid from the plasma sample was performed by calibration curve and using external standard. Key words: HPLC,...
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Blažková, Petra. "HPLC analýza léčiv III." Master's thesis, 2010. http://www.nusl.cz/ntk/nusl-282925.
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ANALYTICAL EVALUATION OF ACTIVE SUBSTANCE BY LIQUID CHROMATOGRAPHY II. Diploma thesis Petra Blažková Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové The subject of this diploma thesis is a determination of active substances by liquid chromatography. In particular it deals with an evaluation of phenobarbital in biological matrix. Solid phase microextraction (SPME) and high performance liquid chromatography (HPLC) with UV detector (218 nm) and reversed phase C18 comlumn were used. The mobile phase consisted of methanol and phosphate buffer in a ratio of 50:50. The flow rate was set to 0,4 ml/min. 20 µl of sample solution was injected on the chromatographic column. Phenobarbital was dissolved in a mixture of methanol and buffer in a ratio of 80:20. For the SPME extraction from water solution was used carbowax/TPR fibre. The analyte was desorbed into methanol. The extraction time was 20 minutes. Phenobarbital extraction from rabbit plasma was performed in the same way, but PDMS/DVB fibre instead of carbowax/TPR fibre was used. Phenobarbital in rabbit plasma was quantified by means of calibration curve.
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Štichová, Lucia. "HPLC analýza léčiv IV." Master's thesis, 2012. http://www.nusl.cz/ntk/nusl-307831.
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HPLC analysis of drugs IV. Diploma Thesis Lucia Štichová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové In this thesis, conditions were optimized for high-performance liquid chromatography for quantitative evaluation of ibuprofen. It was established solid phase microextraction conditions for which ibuprofen was extracted from whole blood. The fiber was coated with polydimethylsiloxane - divinylbenzene with a thickness of 60 µm. The fiber was immersed in the sample. The blood sample was adjusted to pH 2.6. Sorption time was set at 30 minutes and the methanol desorption time was 15 minutes. The mobile phase consisted of methanol with water in the ratio 8:2 and pH was adjusted to a value of 3. The flow rate was 1 ml / min and detection was carried out at a wavelength of 222 nm. For quantitative evaluation the external standard was used. The detection limit was 0.005 µg / ml and the quantification limit was 0.017 µg / ml.
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Sochová, Veronika. "HPLC analýza léčiv V." Master's thesis, 2013. http://www.nusl.cz/ntk/nusl-322175.
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HPLC analysis of drugs V Diploma thesis Veronika Sochová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control In this diploma thesis was established the methodology for the evaluation of dexamethasone in biological material using solid phase microextraction and HPLC. For the measurements was used extraction fibre polydimethylsiloxane in combination with divinylbenzene. The fiber was used for microextraction of dexamethasone from water samples and plasma samples. Conditions were optimized for SPME evaluation of dexamethasone and diazepam (internal standard) in plasma sample. Sorption time was 10 minutes, desorption time was 20 minutes to 0,2 ml methanol. Chromatographic conditions - column C18, eluent acetonitrile - water, 55:45 (v/v) and detection at a wavelength of 240 nm.
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Krouská, Hana. "HPLC studie chemických reakcí." Master's thesis, 2015. http://www.nusl.cz/ntk/nusl-342935.
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In this work hydrolysis of phenylisothiocyanate and subsequent decomposition of diphenylthiourea were studied. RP-HPLC with UV detection was selected for monitoring of these reactions. The new method of isocratic elution was developed and mobile phase composition and flow rate were optimized. Hydrolysis of isothiocyanate was studied as a function of pH and reaction temperature. The subsequent decomposition of diphenylthiourea was carried out at 80 řC depending on the pH.
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Žáková, Petra. "Optimalizace HPLC stanovení klotrimazolu." Master's thesis, 2008. http://www.nusl.cz/ntk/nusl-291039.
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High-performance liquid chromatographic technique for the determination of clotrimazole and its degradation products (2-chlorophenyl)-diphenyl methanol and imidazole in the formulation Clotrimazol spray 1 % was developed. The presented thesis was focused to the selection of optimal column, composition of mobile phase, its pH and internal standard for the analysis of pharmaceutical formulation based on topically applied antifungal agent clotrimazole. Seven columns were tested in detail. The tested columns were: Discovery HS F5 (5 μm, 150 x 4.6 mm)Chromolith® Performance, RP-18e (100 x 3 mm)ZIC® HILIC (3.5 μm, 50 x 2.1 mm)XTerra® RP 18 (5 μm, 100 x 3 mm)Discovery RP Amide C 16 (5 μm, 250 x 3 mm)Zorbax Extend-C18 (3.5 μm, 75 x 4.6 mm)Discovery ZR-PBD (5 μm, 150 x 4.6 mm). HPLC was carried out using Discovery ZR- PBD column 5 μm, 150 x 4.6 mm. This column is based on polybutadiene-coated zirconium oxide. A zirconium oxide is stable in the whole pH range with the high pressure and temperature up to 200řC. Spectrophotometric detection at 210 nm was performed. The optimal mobile phase was a mixture of acetonitrile and water (pH 9.7) in the ratio of 50:50. The pH of the water component was finally adjusted to 9.7 with NH4OH 25 %. The aqueous solution was filtered through 0.45 m Millipore...
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Paličková, Karolína. "HPLC stanovení potenciálních léčiv." Master's thesis, 2017. http://www.nusl.cz/ntk/nusl-368250.
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1 ABSTRACT Charles University Faculty of Pharmacy in Hradec Králové Department of Biophysics and Physical Chemistry Candidate: Karolina Palickova Consultant: Ing. Vladimir Kubicek, CSc. Title of Thesis: HPLC Determination of Potencial Drugs The diploma thesis describes selection of the most suitable conditions for HPLC determination of a recently prepared potential bronchodilatans. The aim of the thesis was to find a suitable isocratic method for the HPLC determination of the substance in rat plasma to be used during pharmacokinetic experiments. The chromatographic column Ascentis® Express RP - Amide was utilized. Best results were achieved with mobile phase consisting of acetonitrile and phosphate buffer (pH = 3,0) in volume ratio 12:88. The column was thermostated at 20 řC. Fluorescence detection (λex = 228 nm, λem = 380 nm) was applied to get a sufficient sensitivity. 4-quinazolinole was chosen as an internal standard. Biological samples were processed by LLE before the HPLC analyses. The proposed method was validated successfully and then employed in pharmacokinetic studies.
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Chen, Jing-Fei, та 陳莖斐. "以HPLC分析Enalaprilmaleate". Thesis, 1997. http://ndltd.ncl.edu.tw/handle/18501893499335426628.
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Vyroubal, Petr. "HPLC hodnocení vybraných léčiv II." Master's thesis, 2010. http://www.nusl.cz/ntk/nusl-279050.
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HPLC evaluation of selected drugs II. THESIS Petr Vyroubal Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control In this thesis was validated method for simultaneous HPLC analysis of paracetamol and tramadol in combined tablet. As stationary phase the chromatographic column Discovery HS F5, 5 µm, 150×3 mm I.D. made by Supelco was used. Mobile phase was formed by mixture of acetonitrile : ammonium acetate solution 0.005 mol/l, acidified with acetic acid at pH 3.2 in the ratio 20:80 (v/v). A flow rate was 1.0 ml/min. Acetylsalicylic acid was used as an internal standard. The detection was performed at λ = 270 nm using an UV detector. The substances were eluted in following order: paracetamol, acetylsalicylic acid and tramadol. The method was validated for linearity (paracetamol R = 0.9996; tramadol R = 0.9998), precision (paracetamol RSD = 0.31 %; tramadol RSD = 0.70 %), accuracy (paracetamol recovery = 99.49 %; tramadol recovery = 98.90 %) and robustness.
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Skryjová, Denisa. "HPLC hodnocení vybraných léčiv I." Master's thesis, 2010. http://www.nusl.cz/ntk/nusl-279106.
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61 ABSTRACT HPLC evaluation of selected drugs I. THESIS Denisa Skryjová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control In this thesis were developed the optimum chromatographic conditions for simultaneous HPLC analysis of tramadol and paracetamol in combined tablet. The chromatographic column Discovery HS F5, 5 µm, 150×3 mm I.D. made by Supelco was chosen as the stationary phase. Mobile phase mixture formed acetonitrile : ammonium acetate solution 0.005 mol/l, acidified with acetic acid at pH 3.2 in the ratio 20:80 (v/v), at a flow rate of 1.0 ml/min. Acetylsalicylic acid was used as an internal standard. Detection took place at λ = 270 nm using a UV detector. The compounds were eluted in order of paracetamol, acetylsalicylic acid and tramadol.
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Šestakova, Veronika. "Využití HPLC ve farmaceutické analýze." Master's thesis, 2009. http://www.nusl.cz/ntk/nusl-279512.
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Determination of hexachlorophene in the product SEPTONEX ointment to the Department of Analytical Chemistry performed by HPLC. This method has many advantages over previously used titrate determination. The conditions of analysis are as follows: mobile phase is composed of 85% methanol with the addition of 1% acetic acid, column Purospher Merck RP C18, 5 mm (12.5 cm x 4 mm), flow rate of the mobile phase is 1.5 ml / min, sample injection volume is 20 µl. The aim was to optimize the use of methods, i.e. find the column using the modern trends in HPLC, which would allow obtaining precise, rapid and well reproducible results under similar chromatographic conditions. Based on the literature research were selected six different analytical columns with more or less similar characteristics as the column still used. In each of these columns have been measured solutions of standards hexachlorophene and solutions of ointment SEPTONEX samples at different flow rate of mobile phase. Other conditions of analysis have been retained. From the experiment showed that the tested columns is the most appropriate column Chromolith Performance RP18-e (10 cm x 4,6 mm) at a flow rate of mobile phase 2.0 ml / min. Another challenge was to find a suitable internal standard for faster and more accurate determination of...
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Bajcurová, Lucie. "Využití HPLC ve farmaceutické analýze." Master's thesis, 2010. http://www.nusl.cz/ntk/nusl-279529.
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The HPLC method for determination of ketoprofen in therapeutic preparations "PRONTOFLEX" - a 10% skin spray and "Ketonal" - a 5% cream has been developed. This method was based on already developed and validated method for analyzing the preparation "KETOPROFEN" - a 2.5% gel. Both of the methods have been developed in the same department. The chromatographic separation was performed on SUPELCO Discovery C18 column (125 mm x 4.6 mm, 5 µm). The mobile phase consisted of a mixture of acetonitrile, water and a phosphate buffer pH 3.5 (40:58:2, v/v/v). At a mobile phase flow rate of 1.0 ml/min, injection volume of 10 μl and UV detection at a wavelength of 233 nm, the total time of analysis was less than 10 minutes. Ethylparaben was used as an internal standard.
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Soukupová, Petra. "HPLC hodnocení vybraných léčiv IV." Master's thesis, 2011. http://www.nusl.cz/ntk/nusl-296767.
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HPLC evaluation of some drugs IV. THESIS Petra Soukupová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Analysis This thesis is about looking for the optimal conditions for simultaneous HPLC analysis in combined tablets of perindopril and indapamid with subsequent determination of their content. As the most suitable stacionary phase chromatographic column LiChro CART 250-4 LiChrospher 100, RP18, 5 µm was chosen, and the mobile phase formed by mixture of acetonitrile - ammonium phosphate solution (0,05 mol/l) in the ratio 40:60 with addition of triethylamine (0,1 ml/100 ml) acidified with phosporic acid at pH 3 at a flow rate of 1,4 ml/min and temperature 50o C. Propylparaben was used as the most suitable internal standard. The detection was performed at 215 nm using an UV detector. At the determination of content of medicaments in tablets was found that used compounds were eluted in following order: perindopril, indapamid and propylparaben.
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Kadaňková, Barbora. "HPLC hodnocení vybraných léčiv VI." Master's thesis, 2012. http://www.nusl.cz/ntk/nusl-308214.
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Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate: Barbora Kadaňková Consultant: RNDr. Milan Mokrý, CSc. Title of Thesis: HPLC hodnocení vybraných léčiv VI. This thesis focuses on assay optimization for simultaneous quantitation of valsartan and hydrochlorothiazide in combined tablets. First, chromatographic conditions were tested and optimized settings were then used for tablet content determination. Good chromatographic separation was achieved using an ET Nucleosil (125x4.6 mm, 120-5, C8) column and a mobile phase consisting of acetonitrile : ammonium acetate (0.001 mol/l) in the ratio of 25:75 (v/v) with addition of sodium hexanesulfonate (0.002 mol/l). The solution was acidified with acetic acid to pH 3.50 and then adjusted to pH 7.00 using disodium hydrogen phosphate. The mobile phase was pumped at a flow rate of 1.0 ml/min and UV detector was set at 254 nm. Methylparaben was used as internal standard. Individual compounds eluted in the following order: 1) hydrochlorothiazide, 2) valsartan and 3) methylparaben. The linearity range for valsartan and hydrochlorothiazide quantitation was 0.08-0.24 mg/ml and 0.012-0.036 mg/ml, respectively.
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Kašková, Jana. "HPLC hodnocení vybraných léčiv V." Master's thesis, 2012. http://www.nusl.cz/ntk/nusl-308261.
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Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate: Jana Kašková Consultant: RNDr. Milan Mokrý, CSc. Title of Thesis: HPLC evaluation of some drugs V. This thesis is about looking for the optimal conditions for simultaneous HPLC analysis in combined tablets of amlodipin and atorvastatin with subsequent determination of their content. As the most suitable stacionary phase was chosen chromatographic column 125x4 mm I. D. contains Nucleosil 120-5 C 18, Macherey-Nagel, and the mobile phase formed by mixture of acetonitrile - disodium hydrogen phosphate dodecahydrate solution (0,025 mol/l) in the ratio 55:45, acidified with phosporic acid at pH 4,4 at a flow rate of 1,0 ml/min and temperature 25řC. Propylparaben was used as the most suitable internal standard. The detection was performed at 210 nm using an UV-VIS detector. At the determination of content of medicaments in tablets was found that used compounds were eluted in following order: propylparaben, atorvastatin and amlodipine besylate.
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Hynková, Martina. "HPLC hodnocení vybraných léčiv VIII." Master's thesis, 2014. http://www.nusl.cz/ntk/nusl-333273.
Full textAbstract:
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Student: Martina Hynková Supervisor: RNDr. Milan Mokrý, CSc. Diploma thesis: HPLC evaluation of selected pharmaceuticals VIII RP-HPLC method for simultaneous analysis of Paracetamol, Ascorbic Acid and Phenylephrine in pharmaceutical formulation (powder for oral solution) was developed. In this formulation, the amount of Paracetamol is sixtimes higher then the amount of Phenylephrine. Macherey-Nagel column NUCLEOSIL C18 (150 mm x 4 mm id, 5 µm particle size) was used as a sorbent. Isocratic elution with mobile phase composed of 0,001M monopotassium phosphate puffer and organic modifier methanol (80 : 20, V/V; pH 3,00 - adjusted with 50% phosphoric acid) at a flow rate of 0,7 ml.min-1 and 25 řC in less then 14 minutes. UV detection at the wavelenght 225 nm. Sample volume 10 µl. The influence of variations in mobile phase parameters (pH, content of organic modifier and puffer concentration) was observed. With allopurinol as an IS, calibration was performed to enable quantification of drugs in pharmaceutical formulation.
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Pleváková, Magdaléna. "Stanovení lipofility léčiv pomocí HPLC." Master's thesis, 2015. http://www.nusl.cz/ntk/nusl-339515.
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3 ABSTRACT Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of biophysics and physical chemistry Author: Magdaléna Pleváková Supervisor: Ing. Vladimír Kubíček, CSc. Thesis title: Determination of Lipophilicity of Drugs by HPLC In this thesis a RP-HPLC method for fast and reliable determination of lipophilicity was proposed and tested. Stationary phase was selected by using hydrophobic substraction model. Capacity factors of the chosen substances were initially measured on Zorbax ECLIPSE XDB C18 250x4,6 mm, 5µm column, which exhibits almost identical retention characteristics as the column used for this purpose until now. Then the capacity factors of the same substances were determined by using Zorbax ECLIPSE XDB-C18 50x4,6 mm, 1,8µm column that was selected to reduce retention times significantly. A group of newly synthesised drugs based on structure of pyrazine served as samples for the measurement. The reproducibility of the capacity factor values determined using both columns was compared and the independence of the capacity factor on the mobile phase flow was confirmed. The capacity factors of two homologous series and a group of benzimidazols were consequently determined on Zorbax ECLIPSE XDB-C18 50x4,6 mm, 1,8µm column using various compositions of mobile phases. Several...
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Kopecká, Iva. "Hodnocení zolpidem - tartarátu pomocí HPLC." Master's thesis, 2016. http://www.nusl.cz/ntk/nusl-344175.
Full textAbstract:
Charles University in Praque, Faculty of Pharmacy in Hradci Králové Department: Pharmaceutical Chemistry and Drug Control Candidate: Iva Kopecká Tutor: PharmDr. Pavla Pilařová, Ph.D. Name of Degree Paper: Evaluation of zolpidem tartrate using HPLC In the diploma thesis, there was optimazed the method of separation of zolpidem tartrate and its impurity A. There was tested the influence of the composition of the mobile phase, molarity of phosphate buffer, its pH and the temperature on the column. The optimal conditions of the separation were determined - methanol:acetonitril: 0,06 mol/l phosphate buffer pH 4 (20:15:65), the temperature on the column 30řC, the flow rate of the mobile phase was 1ml/min and the detection in the UV in the wavelength of 254 nm. Afterwards, the method was used for rating of stability tests in these load conditions - alkaline environment, increased temperature, oxidative environment and daylight. The decrease of the concentration of effective substance of zolpidem tartrate in the given environment and time was observed as well as the potential development of the destructive products of the effective substance.
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Skopový, Štěpán. "HPLC hodnocení vybraných léčiv XI." Master's thesis, 2015. http://www.nusl.cz/ntk/nusl-348613.
Full textAbstract:
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate: Štěpán Skopový Consultant: RNDr. Milan Mokrý, CSc. Title of Thesis: HPLC evaluation of some drugs XI. The main focus of this diploma thesis was to find suitable chromatografic conditions for HPLC analysis of Fenofibrate and Ketorolac. Aproximate chromatographic conditions for analysis of Fenofibrate were suggested based on review of previous research projects concerning HPLC analysis of this drug. As for the stacionary phase, a C18 column (250 x 4.6 mm, 5µm particle size) was considered to be the most suitable. Suggested mobile phase is to be formed by mixture of acetonitrile and phosfate buffer (pH aproximetly 3,6) in the ratio 50: 50 or 60:40. Detection could be carried out by an UV-VIS detector at 286 nm. For the analysis of ketorolac it was used Sigma-Aldrich's Discovery HS C18 HPLC column (150x4.6 mm, 5 μm). The mobile phase consisted of acetonitrile and 0,01 mol/l potassium dihydrogen phosphate buffer (pH 3.25) in the ratio 40:60 (v/v). Isocratic elution at a flow rate of 1 ml/minute was set at temperature 25řC and the maximum pressure was 20 Mpa. Thiaprofenic acid was used as internal standard and the detection was carried out by a PDA detector (model SPD-M20...