Dissertations / Theses on the topic 'HPLC (high-performance liquid chromatography)'
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Benson, Andrew James. "High-performance liquid chromatography (HPLC) and high-performance liquid chromatography mass spectrometry (HPLC/MS) for the analysis of date rape drugs." FIU Digital Commons, 2002. http://digitalcommons.fiu.edu/etd/1602.
Full textEdwardson, P. A. D. "High Performance Liquid Chromatography of polynucleotides and proteins." Thesis, London School of Hygiene and Tropical Medicine (University of London), 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.376534.
Full textForssén, Patrik. "Adsorption isotherm parameter estimation in nonlinear liquid chromatography /." Uppsala : Acta Universitatis Upsaliensis : Univ.-bibl. [distributör], 2005. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-5971.
Full textDONALD, GREGORY THOMAS. "Model Chiral Ionic Liquids for High Performance Liquid Chromatography Stationary Phases." University of Cincinnati / OhioLINK, 2008. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1214325450.
Full textRitchie, Harald John. "Development of new packing materials for high performance liquid chromatography." Thesis, University of Edinburgh, 1987. http://hdl.handle.net/1842/14283.
Full textScholtzova, 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.
Full textWalker, Roderick Bryan. "HPLC analysis and pharmacokinetics of cyclizine." Thesis, Rhodes University, 1995. http://hdl.handle.net/10962/d1003279.
Full textNarine, Raymond. "A novel microcomputer-controlled transport detector for high-performance liquid chromatography." Thesis, King's College London (University of London), 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.281718.
Full textLowe, Christian T. "Retention characteristics of water-soluable calixarene modified mobile phases in HPLC /." Connect to the full text of the document, 1998. http://www.ohiolink.edu/etd/view.cgi?ysu997550028.
Full textLi, F. "Studies of haem biosynthesis and metabolism by high-performance liquid chromatography." Thesis, University of Cambridge, 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.378943.
Full textWatson, Richard Charles. "Studies of reversed phase high performance liquid chromatography (RP-HPLC) stationary phases." Thesis, University of Nottingham, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.338492.
Full textTrusova, Tatyana. "Quantitative estimation of bile acid conjugates in human bile using HPLC /." Connect to online version, 1995. http://hdl.handle.net/1989/3555.
Full textWeddle, Carolyn A. "Optimization of HPLC techniques for separation of oxidized phosphatidylcholines." Virtual Press, 2005. http://liblink.bsu.edu/uhtbin/catkey/1319835.
Full textDepartment of Chemistry
Soor, Amritpal. "Group separation of complex mixtures by normal-phase high performance liquid chromatography and analysis by gas chromatography." [S.l. : s.n.], 2008. http://nbn-resolving.de/urn:nbn:de:bsz:289-vts-64791.
Full textWitte, Dirk Theodoor. "High performance liquid chromatography for direct and indirect enantiomeric separations of chiral drugs." [S.l. : [Groningen : s.n.] ; University Library Groningen] [Host], 1992. http://irs.ub.rug.nl/ppn/297969609.
Full textSexton, Danessa Leann. "Determination of lactose by reversed-phase high performance liquid chromatography." [Johnson City, Tenn. : East Tennessee State University], 2004. http://etd-submit.etsu.edu/etd/theses/available/etd-0328104-212023/unrestricted/SextonD041504f.pdf.
Full textTitle from electronic submission form. ETSU ETD database URN: etd-0328104-212023. Includes bibliographical references. Also available via Internet at the UMI web site.
Ansong, Godfred. "Analysis of plant polyphenols by high performance liquid chromatography/mass spectrometry and protein binding." Oxford, Ohio : Miami University, 2004. http://rave.ohiolink.edu/etdc/view?acc%5Fnum=miami1083081905.
Full textPatel, Hasmukh B. "Reversed-phase high-performance liquid chromatography : some basic studies and application in microbial transformation." Thesis, University of Bath, 1987. https://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.379158.
Full textForage, Nazhat George. "RP-HPLC separation and kinetics of the decomposition products of tryptophan amadori compound." Thesis, McGill University, 1990. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=59880.
Full textKlute, Robert Cragg. "Enantiomeric separations by HPLC : temperature, mobile phase, flow rate and retention mechanism studies /." This resource online, 1993. http://scholar.lib.vt.edu/theses/available/etd-06062008-171241/.
Full text張雅茗. "營實HPLC指紋圖譜研究初探." HKBU Institutional Repository, 2013. http://repository.hkbu.edu.hk/etd_ra/1364.
Full textEliser, Erica E. "Synthesis and Characterization of Amino-derived t-butyl-calix[4]arene Bonded Phases for HPLC." Youngstown State University / OhioLINK, 2001. http://rave.ohiolink.edu/etdc/view?acc_num=ysu1008341180.
Full textSmith, Anita Mohler. "Objective judgement of cheese varieties by multivariate analysis of HPLC profiles." Thesis, University of British Columbia, 1987. http://hdl.handle.net/2429/26535.
Full textLand and Food Systems, Faculty of
Graduate
Dotlich, Erin Michele. "ALKYLAMMONIUM FORMATE IONIC LIQUIDS AS SOLVENTS FOR FLUORESCENCE AND LIQUID CHROMATOGRAPHY METHODS." Miami University / OhioLINK, 2008. http://rave.ohiolink.edu/etdc/view?acc_num=miami1208983119.
Full textHuyghues-Despointes, Alexis. "Synthesis, characterization, and approaches to the analysis by HPLC-THG-AAS of trimethylselenonium, selenoniumcholine and selenoniumacetylcholine cations." Thesis, McGill University, 1991. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=59977.
Full textThe analysis was performed by high performance liquid chromatography with atomic absorption detection. The chromatography on a cynopropyl silica bonded phase was optimized for mobile phase composition by response surface analysis. The resulting surface response plots permitted a differentiation between the mechanisms of action of two mobile phase modifiers: triethylamine and trimethylsulfonium iodide. The improvement in chromatographic efficiency resulted in two to three fold decrease in the limit of detection. An extraction procedure with liquefied phenol was evaluated for the determination, by HPLC-AAS, of traces of selenonium cations in biological samples. The advantages and shortcomings of the HPLC-THG-AAS approach are discussed.
Murphy, Kellyann M. "Analysis of Biodiesel Quality Using Reversed Phase High-Performance Liquid Chromatography." Scholarship @ Claremont, 2012. http://scholarship.claremont.edu/pomona_theses/45.
Full textPalmero, David A. "Comparison of cyclic voltammetry and HPLC for the determination of phenol in over-the counter sore throat sprays /." View abstract, 1999. http://library.ctstateu.edu/ccsu%5Ftheses/1540.html.
Full textThesis advisor: James V. Arena, Ph. D. " ... in partial fulfillment of the requirements for the degree of Master of Science in Chemistry." Includes bibliographical references (leaf 48).
Bottegal, Megan N. "The Development of High Performance Liquid Chromatography Systems for the Analysis of Improvised Explosives." FIU Digital Commons, 2010. http://digitalcommons.fiu.edu/etd/154.
Full textWang, Tongwen. "Hyphenated HPLC-MS technique for analysis of compositional monosaccharides of transgenic corn glycoprotein and characterization of degradation products of diazinon, fonofos and aldicarb in various oxidation systems." Diss., Rolla, Mo. : University of Missouri-Rolla, 2007. http://scholarsmine.mst.edu/thesis/pdf/WangTongwen_09007dcc804e975c.pdf.
Full textVita. The entire thesis text is included in file. Title from title screen of thesis/dissertation PDF file (viewed April 23, 2008) Includes bibliographical references.
Loegel, Thomas N. "High Performance Liquid Chromatography of Petroleum Asphaltenes and Capillary Electrophoresis of Glycosaminoglycan Carbohydrates." Miami University / OhioLINK, 2012. http://rave.ohiolink.edu/etdc/view?acc_num=miami1354241855.
Full textLien, Wan-Fu. "Separation of Transition Metal Ions by HPLC, Using UV-VIS Detection." Thesis, North Texas State University, 1987. https://digital.library.unt.edu/ark:/67531/metadc501145/.
Full textSuen, Kin-wah, and 孫建華. "Validation of a HPLC assay for porphobilinogen synthase in human erythrocytes for use in the clinical laboratory." Thesis, The University of Hong Kong (Pokfulam, Hong Kong), 2004. http://hub.hku.hk/bib/B29624897.
Full textabstract
toc
Medical Sciences
Master
Master of Medical Sciences
Hanan, Nathan, and David Nix. "Extending the Stability of Intravenous Ampicillin." The University of Arizona, 2012. http://hdl.handle.net/10150/614496.
Full textSpecific Aims: To assess the chemical stability of ampicillin for injection in normal saline at pH values ranging from 5 to 6. Methods: A stability-indicating high performance liquid chromatography (HPLC) method was developed and used to determine the stability of ampicillin for injection in normal saline following buffering with sodium acetate and acid adjustment with HCl at pH values of 5, 5.5, and 6. To confirm that the assay was stability-indicating, ampicillin trihydrate reference standard (1 mg/mL) was exposed to alkali, acid, and oxidative stress conditions and analyzed by HPLC for the presence of degradation products. Analysis was performed on a reverse-phase (C-18) column with a mobile phase consisting of water, acetonitrile, 1 M monobasic potassium phosphate, and 1 N acetic acid (909:80:10:1). Other HPLC parameters were: flow rate 1 mL/min; detection wavelength 254 nm; injection volume 20 µL; column temperature 30˚C. The method was evaluated for linearity, precision, and accuracy. The chemical stability of ampicillin for injection (18 mg/mL) in normal saline and sodium acetate (pH adjusted at values of 5, 5.5, and 6) was assessed at baseline (t=0), 7, 11, 17, 31, and 44 hours and compared to a control solution (no pH adjustment). Measurements at each time interval were performed in triplicate. Main Results: Ampicillin trihydrate reference standard (1 mg/mL) was adequately separated from degradation products following exposure to alkali, acid, and oxidative stress conditions. After 16 hours, a precipitate was observed in the solution at pH 6, and therefore stability is not reported. All other solutions (pH 5, pH 5.5, and control) were stable for at least 24 hours at room temperature and yielded t90 values of 110, 64.2, and 27.5 hours, respectively. Conclusions: Adjustment of intravenous ampicillin solutions to pH values of 5 or 5.5 significantly increased stability. Ampicillin appears to be most stable at a pH near its isoelectric point (pH 5).
Li, Cheuk Fai. "Studies of flow injection system for micelle-assisted preconcentration of PAHs coupled with HPLC." HKBU Institutional Repository, 2009. http://repository.hkbu.edu.hk/etd_ra/1059.
Full textMarques, Tamires Valim 1987. "Desenvolvimento e validação de método analítico empregando DLLME e HPLC/UV para determinação de benzodiazepínicos em amostra de água." [s.n.], 2014. http://repositorio.unicamp.br/jspui/handle/REPOSIP/265966.
Full textDissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica
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Resumo: A crescente preocupação com a poluição das águas por novos poluentes denominados emergentes tem se intensificado, visto que aumentou o número destes compostos detectados em água. Dentre estes compostos encontram-se os fármacos e produtos de higiene pessoal, usados cotidianamente pela população. O presente trabalho teve como objetivo o desenvolvimento de um método simples, rápido e sensível utilizando a microextração líquido líquido (DLLME) combinada com a cromatografia líquida de ultra eficiência (HPLC) com detecção ultravioleta (UV) para a determinação de alguns benzodiazepínicos (bromazepam, clonazepam e diazepam) em amostras de água. A determinação foi realizada em uma coluna C18 de acordo com as condições cromatográficas ótimas (fase móvel acetonitrila:água (60:40, v/v); vazão 1,2 mL min-1; detecção 225 nm). No método de extração, uma mistura apropriada de solvente extrator e dispersor foi injetada rapidamente na amostra aquosa (10 mL) com auxílio de uma seringa. De modo que uma solução turva foi formada, esta solução é caracterizada por conter pequenas partículas do solvente extrator que se dispersa na fase aquosa. Os parâmetros da extração, tais como natureza e volume dos solventes extrator e dispersor, tempo de extração, pH da amostra, força iônica, velocidade e tempo de centrifugação, foram estudados para a otimização. Com as condições ótimas definidas (solvente extrator: clorofórmio, 200 ?L; solvente dispersor: metanol, 700 ?L; pH da amostra 9,0; velocidade e tempo de extração: 5000 rpm, 1 minuto; força iônica: adição de 1% (p/v) de (NH4)2SO4) o método proposto foi validado seguindo as figuras de método preconizadas pela ANVISA na Resolução N° 899 de 2003. A faixa linear para cada fármaco foram 8,0 - 96 ?g L-1 para bromazepam, 4,0 - 48 ?g L-1 para clonazepam e 1,0 - 12 ?g L-1 para diazepam. Todas as curvas obtiveram valores de (r) superiores a 0,999. Os limites de detecção e quantificação obtidos foram 2,4 e 8,0 ?g L-1 para bromazepam, 1,2 e 4,0 ?g L-1 para clonazepam, 0,2 e 1,0 ?g L-1 para diazepam, respectivamente. As recuperações variaram de 50 a 110% com RSD (Desvio Padrão Relativo) inferiores a 12,7 %. Finalmente, o método proposto foi aplicado em amostras coletadas na represa Billings localizada no município de Diadema-SP.
Abstract: The growing concern over water pollution caused by so-called new emerging pollutants has intensified since increased the number of these compounds detected in water. Among these compounds are pharmaceuticals and personal care products used daily by the population. This study aimed to develop a simple, rapid and sensitive liquid using liquid micro extraction (DLLME) combined with ultra-performance liquid chromatography (HPLC ) with ultraviolet detection (UV) for the determination of some benzodiazepines (bromazepam, clonazepam and diazepam) in water samples . The determination was performed on a C18 column in accordance with the optimal chromatographic conditions (mobile phase acetonitrile: water (60:40, v/v), flow rate 1.2 mL min-1, detection 225 nm). In the extraction method, a suitable mixture of extractant and dispersing solvent was injected rapidly into the aqueous sample (10 ml) with a syringe. So that a cloudy solution was formed, this solution is characterized by containing fine drops of the extractor solvent is dispersed in the aqueous phase. The parameters of the extraction, such as the nature and volume of the extractor and disperser solvents, extraction time, sample pH, ionic strength, speed and time of centrifugation, were studied for optimization. With the defined optimal conditions (extracting solvent: chloroform, 200 ?L; disperser solvent: methanol, 700 ?L, sample pH 9.0, extraction time and speed: 5000 rpm, 1 minute; ionic strength: adding 1% (p/v) (NH4)2SO4) the proposed method was validated following the figures of merit recommended by the ANVISA Resolution No. 899 of 2003. The linear ranges for each drug were 8.0 to 96 ?g L- 1 for bromazepam, 4.0 to 48 ?g L- 1 for clonazepam and 1.0 to 12 ?g L- 1 for diazepam. All curves obtained values (r) greater than 0.999. The limits of detection and quantification obtained were 2.4 and 8.0 ?g L- 1 to bromazepam, 1.2 and 4.0 ?g L- 1 to clonazepam, 0.2 and 1.0 ?g L- 1 for diazepam, respectively. Recoveries ranged from 50 to 110% with RSD (Relative Standard Deviation) of less than 12.7%. Finally, the proposed method was applied to samples collected in the Billings dam located in Diadema-SP.
Mestrado
Materiais e Processos de Fabricação
Mestre em Engenharia Mecânica
Wang, Yu. "HPLC method development for the evaluation of pheromones from the dwarf African clawed frog Hymenochirus." Scholarly Commons, 2003. https://scholarlycommons.pacific.edu/uop_etds/587.
Full textHayteas, David Lawrence. "HPLC analysis of myoglobin tryptic peptides from selected species of cetaceans." PDXScholar, 1990. https://pdxscholar.library.pdx.edu/open_access_etds/4086.
Full textVan, Meter David S. III. "Synthesis and Characterization of Surface-Confined Ionic Liquid Stationary Phases for High Performance Liquid Chromatography." University of Cincinnati / OhioLINK, 2008. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1227275073.
Full textPerdue, James D. "The removal of Cremophor® EL from paclitaxel for quantitative analysis by HPLC-UV /." Electronic version (PDF), 2005. http://dl.uncw.edu/etd/2005/perduej/jamesperdue.pdf.
Full textCollins, Matthew P. "Reversed Phase Liquid Chromatography Using the Ionic Liquid Isopropylammonium Formate and Comparison of Indirect Spectrophotometric Methods for Phosphate." Miami University / OhioLINK, 2011. http://rave.ohiolink.edu/etdc/view?acc_num=miami1312342055.
Full textAlmassalkhi, Brittany A. "Arsenic Speciation, Detection, and Quantification in Drinking Water using High Performance Liquid Chromatography and Inductively Coupled Plasma Mass Spectrometry." University of Cincinnati / OhioLINK, 2009. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1258580087.
Full textBrannegan, Daniel Robert. "Analysis of Ethoxyquin and its Oxidation Products using Supercritical Fluid Extraction and High Performance Liquid Chromatography with Chemiluminescent Nitrogen Detection." Thesis, Virginia Tech, 2000. http://hdl.handle.net/10919/31575.
Full textMaster of Science
Kamble, Ujjwala Kerba. "Use of liquid chromatography for assay of flavonoids as key constituents and antibiotics as trace elements in propolis : investigation into the application of a range of liquid chromatography techniques for the analysis of flavonoids and antibiotics in propolis, and extraction studies of flavonoids in propolis." Thesis, University of Bradford, 2016. http://hdl.handle.net/10454/14564.
Full textNascimento, DemÃtrius Fernandes do. "Nimodipine determination in human plasma by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS-MS)." Universidade Federal do CearÃ, 2005. http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=31.
Full textA rapid, specific and highly sensitive liquid chromatography-tandem mass spectrometry method was developed to determine nimodipine in human plasma using dibucaine as the internal standard (IS) is described. The analyte (m/z 418,6 > 342,6) and IS (m/z 344,2 > 271,0) were extracted from plasma samples by liquid-liquid extraction using hexane-ethyl acetate (1:1v/v). Chromatography was performed on a Varian Polaris C18 analytical column (3 micrometer, 50 x 2,0 mm) and pre-column SecurityguardTM C18 (4,0 x 3,0 mm). The phase mobile consisted of Acetonitrile-Ammonium acetate 0.02 ml/L (80:20v/v). The method had a chromatographic run time of 4.5 min and linear calibration curve over the range 0.1- 40 ng/mL (r2 > 0.9938). The limit of quantification (LQ) was 0.1 ng/mL. The intra-day precision for the limit quantification was 0.00% (batch 01), 5.71% (batch 02) and 5.27% (batch 03); for the quality controls low (QCL), middle (QCM) and high (QCH) the results were respectively 8.57, 0.81 and 1.37%. The inter-day precision for LQ and QCL, QCM and QCH were respectively: 7% and 5.46, 4.12 and 3.37%. The intra-day accuracy for LQ was 110, 96 and 104%; for QCL, QCM and QCH the results were100.67, 109.09 and 109.72% respectively. The results of the inter-day accuracy for LQ, QCL, QCM and QCH were respectively and 110.0, 96.0, 104.0% for the limit of quantification and 8.57, 0.81, 1.37% and 100.67, 109.09, 109.72% respectively: 103% e 102.89, 106.60, 109.69%. This validated method was successfully applied for the pharmacokinetic profiles of nimodipine tablets administered to 24 healthy volunteerâs participant of bioavailability comparative study. Geometric mean of Test formulation/Refernce formulation individual percent ratio was 104,56% for AUC0-48h and 55,73% for Cmax. The 90% for the confidence intervals (CI) were 94,80-115,32% e 44,73-69,42%, respectively. The values of half-life and Cmax for test formulation and reference formulation were 27,83;32,78h and 9,48;18,76ng/mL, respectively. The values of Tmax were 2,34;0,98h for the formulations test and reference respectively. Since the 90% CI for Cmax and AUC0-48h, were within the 80-125% interval proposed by the âFood and Drug Administrationâ and ANVISA, it was concluded that the two formulations of nimodipine 30mg tablets were not bioequivalent, according to the rate of absorption after single dose administration.
Um mÃtodo rÃpido, sensÃvel e especÃfico de Cromatografia LÃquida de Alta EficiÃncia acoplada à Espectrometria de Massa (LC-MS-MS) foi desenvolvido para determinar nimodipino (analito) em plasma humano usando dibucaÃna como padrÃo interno (PI). O analito (m/z 418,6 > 342,6) e o PI (m/z 344,2 > 271,0) foram extraÃdos de amostras de plasma atravÃs de extraÃÃo lÃquido-lÃquido utilizando hexano-acetato de etila (1:1v/v). As corridas cromatogrÃficas foram executadas utilizando-se uma coluna analÃtica Varian Polaris C18 (3 micrÃmetros, 50 x 2,0 mm) e uma prÃ-coluna SecurityguardTM C18 (4,0 x 3,0 mm). A fase mÃvel consistiu de acetonitrila-soluÃÃo de acetato de amÃnio 0,02 mol/L (80:20v/v). O mÃtodo teve um tempo total de corrida de 4,5 min e uma curva de calibraÃÃo linear que variou de 0,1-40 ng/mL. O limite de quantificaÃÃo de 0,1 ng/mL. A precisÃo intra-ensaio para o limite de quantificaÃÃo (LQ) foi 0,00% (lote 01), 5,71% (lote 02) e 5,27% (lote 03); para os controles de qualidade baixo (CQB), mÃdio (CQM) e alto (CQA) os resultados foram respectivamente: 8,57, 0,81 e 1,37%. A precisÃo interensaio para o LQ e os CQB, CQM e CQA foram respectivamente de: 7% e 5,46, 4,12 e 3,37%. A exatidÃo intra-ensaio para o LQ foi 110, 96 e 104%; para CQB, CQM e CQA os resultados foram 100,67, 109,09 e 109,72% respectivamente. Os resultados da exatidÃo interensaio para o LQ, CQB, CQM e CQA foram respectivamente de: 103% e 102,89, 106,6, 109,69%. Este mÃtodo foi aplicado para a avaliaÃÃo do perfil farmacocinÃtico do nimodipino administrado em 24 voluntÃrios sadios participantes de um estudo de biodisponibilidade comparativa. A mÃdia geomÃtrica da FormulaÃÃo teste/FormulaÃÃo referÃncia para as porcentagens individuais foi 104,56% para ASC0-48h e 55,73% para Cmax. Os intervalos obtidos a partir do intervalo de confianÃa (IC) de 90% foram 94,80-115,32% e 44,73-69,42% respectivamente. Os valores de meia-vida e Cmax para as formulaÃÃes teste e referÃncia foram de 27,83;32,78h e 9,48;18,76ng/mL, respectivamente. Os valores de Tmax foram de 2,34;0,98h para as formulaÃÃes teste e referÃncia, respectivamente. Considerando o IC de 90% para Cmax e ASC0-48h dentro da variaÃÃo de 80-125% proposto pelo Food and Drug Administration e ANVISA, as duas formulaÃÃes de nimodipino 30mg nÃo sÃo bioequivalentes quanto à taxa de absorÃÃo (Cmax) apÃs uma Ãnica administraÃÃo.
Rösemann, G. M. "Analysis of pyrrolizidine alkaloids in Crotalaria species by HPLC-MS/MS in order to evaluate related food health risks." Electronic thesis, 2006. http://upetd.up.ac.za/thesis/available/etd-08032007-170633/.
Full textPane, Daniela de Queiroz 1977. "Desenvolvimento, validação e aplicação de metodologia para determinação de edulcorantes por HPLC." [s.n.], 2012. http://repositorio.unicamp.br/jspui/handle/REPOSIP/254271.
Full textTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: Foi desenvolvido um novo método, eficiente e econômico, para a análise simultânea de cinco edulcorantes em alimentos (acessulfame-k, sacarina, ciclamato, aspartame e neotame) pela técnica de cromatografia líquida de alta eficiência (HPLC). O método foi validado e aplicado em diferentes produtos da categoria "light¿, "diet¿ e "zero¿, sendo esses refrigerantes, néctares, pós para preparo de refresco, pudins, cappuccinos, achocolatados, geléias, gelatina, molho tipo "barbecue¿, catchup e adoçantes de mesa. Para tanto, utilizou-se uma coluna C18, fase móvel composta por fase aquosa (5 mM de tampão fosfato de sódio monobásico; pH 7) e fase orgânica (acetonitrila), eluição por gradiente, vazão de 0,4 mL.min-1 e temperatura de 56ºC. Os edulcorante apresentaram adequada linearidade na faixa de trabalho. A repetitividade, a precisão intermediária e os limites de detecção e de quantificação foram adequados para os cinco edulcorantes. As taxas de recuperação variaram entre 85,2% e 101,4%, para as diferentes matrizes avaliadas. O método apresentou uma limitação para as amostras contendo cacau, onde não foi possível determinar o ciclamato em virtude da presença de um interferente. Até três edulcorantes utilizados em combinação foram encontrados nas amostras, sendo acessulfame-k e aspartame os mais comumente empregados. As amostras de pudim sabor chocolate, molho tipo "catchup¿ e molho tipo "barbecue¿ apresentaram concentrações de edulcorantes acima do permitido pela legislação brasileira. As amostras de refrigerante sabor limão, sabor guaraná, tipo cola e de refresco em pó, embora estivessem atendendo a legislação, apresentaram teor de edulcorantes acima do declarado no rótulo. O método desenvolvido por HPLC foi comparado a uma metodologia por cromatografia líquida de ultra eficiência (UPLC) e apresentou maior robustez e menor custo em comparação ao desenvolvimento para UPLC. Já o método por UPLC demonstrou baixo consumo de solventes, tempo curto de análise, menores limites de detecção e de quantificação, no entanto, maior custo devido ao preparo das amostras e à coluna, solventes, reagentes e filtros envolvidos nas análises
Abstract: We developed a new method, efficient and economical, for the simultaneous analysis of five sweeteners in foods (acesulfame K, saccharin, cyclamate, aspartame and neotame) technique for high performance liquid chromatography (HPLC). The method was validated and applied to different products in the "light", "diet" and "zero", and these soft drinks, nectars, powders for preparation of soft drinks, puddings, cappuccino, chocolate, jams, jelly, sauce type "barbecue" , ketchup and tabletop sweeteners. To both, we used a C18 column, mobile phase consisting of aqueous phase (5 mM sodium phosphate buffer monobasic; pH 7) and organic phase (acetonitrile), gradient elution, flow of 0.4 mL.min-1 and temperature of 56 º C. The sweetener showed acceptable linearity in the range of work. The repeatability, intermediate precision and limits of detection and quantification were adequate for the five sweeteners. Recovery rates ranged between 85.2% and 101.4% for the different matrices evaluated. The method has a limitation for samples containing cocoa, which was not possible to determine cyclamate because of the presence of an interferer. Up to three sweeteners used in combination were found in the samples, with aspartame and acesulfame-k the most commonly employed.Samples of chocolate pudding flavored sauce like "ketchup" sauce like "barbecue" sweeteners showed concentrations above those permitted by Brazilian law. Samples of lemon-flavored soda, flavored guarana, cola and powdered drink mixes, although they were given the rules presented above sweeteners content declared on the label. The method developed HPLC method was compared to an ultra performance liquid chromatographic efficiency (UPLC) and showed greater robustness and lower cost compared to developing for UPLC. Have the method by UPLC demonstrated low consumption of solvents, short time of analysis, lower limits of detection and quantification, however, higher cost due to preparation of samples and the column, solvents, reagents and filters involved in the analyzes
Doutorado
Ciência de Alimentos
Doutor em Ciência de Alimentos
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