Este estudo teve como objetivo desenvolver e validar micrométodo simples e sensível para quantificação de cefuroxima plasmática utilizando CLAE-UV com a finalidade de aplicação no monitoramento das concentrações de cefuroxima de pacientes submetidos à cirurgia de revascularização do miocárdio (RM) com CEC no esquema de doses administradas em bolus. Os tempos de retenção para o fármaco e padrão interno (guaifenesina) foram 5,3 e 8,7 minutos respectivamente, com um tempo de corrida de 15 minutos, utilizando coluna de fase reversa C18 (25 cmX4,6 mm, 5 micra) e fase móvel binária constituída de tampão acetato de amônio e trietilamina 0,025 M pH 4,2 e acetonitrila (80:20, v/v), fluxo de 1,0 mL/min, detecção no ultravioleta, λ=274nm em sistema isocrático de eluição. A validação deste método analítico investigada através dos limites de confiança apresentou sensibilidade de 0,1 µg/mL (LD) e limite inferior de quantificação (LIQ) de 0,20 µg/mL, linearidade na faixa compreendida 0,2 µg/mL a 200 µg/mL e 4,37% e 2,95% para precisão intra- e inter-dias, respectivamente. Boa exatidão (98,75%) e alta seletividade foram registradas para o método. Através de um protocolo de estudo para antibioticoprofilaxia das infecções cirúrgicas investigaram-se dez pacientes com indicação de cirurgia eletiva de revascularização do miocárdio com circulação extracorpórea. Realizou-se o monitoramento das concentrações plasmáticas após a dose de ataque de 1,5 g, seguido da manutenção realizada através de bolus em tres doses de 0,75 g 6/6 horas. Uma vez que as concentrações plasmáticas de cefuroxima obtidas na sexta hora (vale) foram inferiores à recomendada 16 µg/mL (4x MIC), recomenda-se o aumento de 0,75 g 6/6 horas para 1,5 g mantendo-se o intervalo entre doses de forma a atingir aquela requerida na antibioticoprofilaxia das cirurugias cardíacas. / The objective of the study was to validate na analytical method to determine cefuroxime in plasma by high performance liquid chromatography (HPLC - UV) for clinical purposes in surgical patients submitted to elective cardiac surgery of myocardial revascularization with cardiopulmonary bypass after drug administration as IV boluses. Retention times for the analite and its internal standard (guaifenesin) were 5.3 and 8.7 minutes, respectively; run time was 15 minutes, using a reversed phase colunm C18 (250X4.6 mm, 5 micron) and a binary mobile phase of ammonium acetate/trietilamine 0.025 M pH 4.2 and acetonitrile (80:20, v/v), flow rate 1 mL/min, ultraviolet detector, λ=274nm isocratic elution system. Validation of confidence limits presented 0.1 µg/mL sensitivity (LD) and lower limit of quantification (LLOQ) of 0.20 µg/mL, linearity in the range 0.2 µg/mL to 200 µg/mL and 4.37% e 2.95% for intra- / interday precisions, respectively. Good accuracy (98.75%) and high selectivity were obtained. The study protocol for antibiotic prophylaxis of surgical infections was designed for ten patients with indication of elective cardiac surgery of myocardial revascularization with cardiopulmonary bypass. Loading dose of 1.5 g followed by maintenance dose of 0.75 g every six hours by IV boluses were applied and plasma drug monitoring was done. Based on data obtained cefuroxime plasma concentrations at time dose interval were lower than 16 µg/mL (4x MIC) at the trough, consequently it is recommended to increase the maintainance dose from 0.75 g 6/6 h up to 1.5 g 6/6h, to reach the minimum required for the antibiotic prophylaxis of cardiac surgeries.

A obesidade é uma doença crônica que atinge uma parcela preocupante da população mundial. É classificada pela OMS em graus l, ll e lll, de acordo com o Índice de Massa Corporal (IMC). A obesidade Grau lll, ou obesidade mórbida, é um fator agravante para inúmeras doenças crônicas como as doenças gastro-esofágicas, diabetes mellitus e câncer. A cirurgia bariátrica é uma intervenção bastante eficaz quando se fala em obesidade grau lll clinicamente severa. Porém, esta intervenção pode alterar a absorção e biodisponibilidade de fármacos como o inibidor da bomba de prótons, o omeprazol. O objetivo deste estudo foi desenvolver um método analítico sensível e rápido utilizando cromatografia líquida de alta eficiência (CLAE) acoplada a detector de ultra-violeta (UV) para quantificação de omeprazol em plasma de pacientes submetidos a cirurgia bariátrica no pré e pós-operatório. A preparação da amostra foi feita por extração em fase sólida utilizando uma coluna SPE DSC-18Lt. Com coluna cromatográfica Nucleosil standard C18 phases 250 x 4 mm, 5 µm e fase móvel tampão fosfato 50 mM pH 7,0:acetonitrila:metanol (60,5:35:4,5 (v/v/v)). As amostras foram analisadas e os resultados expressos em ng/mL. O método foi validado quanto à sensibilidade, linearidade, seletividade (especificidade), exatidão, precisão, limite de quantificação e robustez. A linearidade encontrada para o método foi de 5 a 1250 ng/mL. O limite de detecção estabelecido foi de 2 ng/mL e o de quantificação de 5 ng/mL. A metodologia apresentou valores de recuperação acima de 90%, exatidão e precisão interensaio variou de 96,5 a 98,1% e 5,4 a 7,0%, respectivamente. A precisão e exatidão intra-ensaio variou de 97,1 a 107,4%, respectivamente. A especificidade do método foi determinada para os seguintes interferentes: pantoprazol, metformina, fenformina, hidroclorotiazida, diazepam, lorazepam, oxazepam, clonazepam, ranitidina, propanolol, claritromicina e sulfametoxazol. A metodologia desenvolvida mostrou ser rápida e eficiente na correlação das concentrações plasmáticas do omeprazol administrado aos pacientes bariátricos, demonstrando uma porcentagem, estatisticamente significativa, na diminuição da absorção do fármaco no pós-operatório. / Obesity is a chronic disease that affects an alarming proportion of the population. This disease is classified by the WHO in grades l, ll and lll, according to the Body Mass Index (BMI). Grade lll obesity or morbid obesity, is an aggravating factor for innumerous chronic diseases such as gastro-esophageal diseases, diabetes mellitus and cancer. Bariatric surgery is a very effective intervention when it comes to clinically severe obesity class lll. However, this intervention can alter the absorption and bioavailability of drugs such as the proton pump inhibitor omeprazole. The objective of this study was to develop a sensitive and rapid analytical method using high performance liquid chromatography (HPLC) coupled to a ultra-violet detector (UV) for quantification of omeprazole in plasma of patients undergoing bariatric surgery before and after the procedure. Sample preparation was performed by solid phase extraction using a DSC-18Lt SPE column. Using a Nucleosil standard C18 phases 250 x 4 mm 5 µm column, mobile phase phosphate buffer 50 mM pH 7.0:acetonitrile:methanol in the proportions of 60.5:35:4.5 (v/v/v), samples were analyzed and the results expressed in ng/ml. The method was validated for sensitivity, linearity, selectivity (specificity), accuracy, precision, quantification limit and robustness. The linearity of this method ranged between 5 and 1250 ng/mL. The detection limit was set at 2 ng/mL and the quantification limit at 5 ng/mL. The methodology presented recovery values above 90%. Inter-assay accuracy and precision ranged from 96.5 to 98.1% and from 5.4 to 7.0%, respectively, while intra-assay accuracy and precision varied from 97.1 to 107.4 and from 2.8 to 4.1%, respectively. The specificity of the method was determined for the following interferers: pantoprazole, metformin, phenformin, hydrochlorothiazide, diazepam, lorazepam, oxazepam, clonazepam, ranitidine, propranolol, clarithromycin and sulfamethoxazole. The developed methodology proved to be fast and effective in correlating the plasmatic concentrations of omeprazole administered to patients undergoing surgery, demonstrating statistically significant percentage in the drug absorption decrease after surgery.

Copaifera langsdorffii (Fabaceae, Caesalpinioideae), conhecida popularmente como \"copaíba\", \"copaibeira\" ou \"pau d\'óleo\", é uma árvore de grande porte que se encontra amplamente distribuída pelo Brasil, desde a floresta amazônica até a vegetação do cerrado. A oleorresina, constituída principalmente por sesquiterpenos e diterpenos, é utilizada na medicina popular no tratamento de desordens infecciosas e inflamatórias. Por outro lado, estudos sobre suas folhas, as quais são constituídas majoritariamente por flavonoides e derivados galoilquínicos, são escassos. Assim, foi proposto o isolamento de marcadores químicos, desenvolvimento e validação de método analítico por CLAE-UV-DAD, bem como o estudo sazonal. O extrato bruto obtido das folhas foi particionado com solventes de polaridade crescente: diclorometano, acetato de etila e n-butanol. As frações em n-butanol e aquosa apresentaram, majoritariamente, compostos polares, dentre os quais se destacaram os derivados galoilquínicos. Para isolamento desses compostos utilizaram-se a cromatografia de permeação em gel de Sephadex LH-20 e a cromatografia líquida de alta eficiência preparativa. Nas análises por CLAE-UV-DAD empregou-se coluna analítica Synergi Polar-RP (100 mm x 3,0 mm, 2,5 ?m) e fase móvel composta por ácido fórmico-água (0,1:99,9, solvente A) e isopropanol- metanol-acetonitrila (0,5:4:6, solvente B). O gradiente de eluição foi A:B (90:10 para 85:15) em 8,33 minutos, seguido por A:B (85:15 para 64:36) até 29,17 minutos, utilizando vazão de 0,68 mL/min. Os estudos de sazonalidade foram realizados com 10 acessos de C. langsdorffii cultivados no Sítio Beija-Flor (Cajuru/SP). A partir da fração aquosa foram isolados e identificados 16 derivados galoilquínicos: ácido 5\'-O-metil-3-Ogaloilquínico (AGQ-1), ácido 5\'\'-O-metil-3,4-di-O-galoilquínico (AGQ-2), ácido 5\',5\'\'-di-Ometil- 3,4-di-O-galoilquínico (AGQ-3), ácido 3,4-di-O-galoilquínico (AGQ-4), ácido 5\'\'-Ometil- 3,5-di-O-galoilquínico (AGQ-5), ácido 5\'-O-metil-3,5-di-O-galoilquínico (AGQ-6), ácido 5\'-O-metil-3,4-di-O-galoilquínico (AGQ-7), ácido 5\',5\'\'-di-O-metil-3,5-di-Ogaloilquínico (AGQ-8), ácido 5\',5\'\'-di-O-metil-4,5-di-O-galoilquínico (AGQ-9), ácido 3,5-di- O-galoilquínico (AGQ-10), ácido 4,5-di-O-galoilquínico (AGQ-11), ácido 5\'-O-metil-4,5-di- O-galoilquínico (AGQ-12), ácido 5\'\'-O-metil-4,5-di-O-galoilquínico (AGQ-13), ácido 3,4,5- tri-O-galoilquínico (AGQ-14), ácido 5\'\'-O-metil-3,4,5-tri-O-galoilquínico (AGQ-15), ácido 5\',5\'\',5\'\'\'-tri-O-metil-3,4,5-tri-O-galoilquínico (AGQ-16). Além disso, por meio das análises realizadas por CLAE-EM foi possível constatar a presença de outros 10 derivados galoilquínicos: ácido 3-O-galoilquínico, ácido 4-O-galoilquínico, ácido 5-O-galoilquínico, ácido 5\'-O-metil-4-O-galoilquínico, ácido 5\'-O-metil-5-O-galoilquínico, ácido 5\'-O-metil- 3,4,5-tri-O-galoilquínico, ácido 5\'\'\'-O-metil-3,4,5-tri-O-galoilquínico, ácido 5\',5\'\'-di-Ometil- 3,4,5-tri-O-galoilquínico, ácido 5\',5\'\'\'-di-O-metil-3,4,5-tri-O-galoilquínico, ácido 5\'\',5\'\'\'-di-O-metil-3,4,5-tri-O-galoilquínico. O método analítico mostrou-se adequado para quantificação de nove derivados galoilquínicos (AGQ-1, AGQ-5, AGQ-6, AGQ-7, AGQ-8, AGQ-9, AGQ-10, AGQ-15, AGQ-16) e dois flavonoides, quercitrina e afzelina, frente aos parâmetros seletividade, linearidade, sensibilidade, precisão e exatidão. Por meio de análise estatística multivariada dos estudos sazonais concluiu-se que os acessos apresentaram perfis químicos qualitativos e quantitativos semelhantes nas coletas isoladas e perfis quantitativos diferentes ao longo dos meses. / Copaifera langsdorffii (Fabaceae, Caesalpinioideae), popularly known as \"copaíba\", \"copaibeira\" or \"pau d\'oleo\", is a large tree widely distributed in Brazil, from Amazon rainforest to savannah vegetation. Its oleoresin, composed mainly of sesquiterpenes and diterpenes, is widely used in folk medicine to treat inflammatory and infectious disorders. On the other hand, studies about its leaves, composed mainly of flavonoids and galloylquinic acid derivatives, are scarce. Therefore, it was proposed to isolate leaves major compounds, to develop and validate an analytical method by HPLC-UV-DAD, as well as to udertake seasonal studies. The crude extract of the leaves was partitioned with solvents of increasing polarity: dichloromethane, ethyl acetate and n-buthanol, in sequence. Chemical profiles of n-buthanol and aqueous fractions showed to be composed of polar compounds, especially galloylquinic acid derivatives. These compounds were isolated by gel permeation chromatography using Sephadex LH-20 and preparative high-performance liquid chromatography. The HPLC-UV-DAD analyses were carried out on a Synergi Polar-RP (100 x 3.0 mm, 2.5 ?m) column. The mobile phase was made up of formic acid-water (0.1:99.9, solvent A), and isopropanol-methanol-acetonitrile (0.5:4:6, solvent B). The elution gradient was A:B (90:10 to 85:15) in 8.33 minutes, followed by A:B (85:15 to 64:36) up to 29.17 minutes using a flow rate of 0.68 mL/ min. The seasonal studies were performed from 10 C. langsdorffii accesses grown on Beija-Flor farm (Cajuru/SP). From the aqueous fraction it was isolated and identified 16 galloylquinic acid derivatives: 5\'-O-methyl-3-Ogalloylquinic acid (GQA-1), 5\'\'-O-methyl-3,4-di-O-galloylquinic acid (GQA-2), 5\',5\'\'-di-Omethyl- 3,4-di-O-galloylquinic acid (GQA-3), 3,4-di-O-galloylquinic acid (GQA-4), 5\'\'-Omethyl- 3,5-di-O-galloylquinic acid (AGQ-5), 5\'-O-methyl-3,5-di-O-galloylquinic acid (GQA-6), 5\'-O-methyl-3,4-di-O-galloylquinic acid (AGQ-7), 5\',5\'\'-di-O-methyl-3,5-di-Ogalloylquinic acid (GQA-8), 5\',5\'\'-di-O-methyl-4,5-di-O-galloylquinic acid (GQA-9), 3,5-di- O-galloylquinic acid (GQA-10), 4,5-di-O-galloylquinic acid (GQA-11), 5\'-O-methyl-4,5-di- O-galloylquinic acid (GQA-12), 5\'\'-O-methyl-4,5-di-O-galloylquinic acid (GQA-13), 3,4,5- tri-O-galloylquinic acid (GQA-14), 5\'\'-O-methyl-3,4,5-tri-O-galloylquinic acid (GQA-15), 5\',5\'\',5\'\'\'-tri-O-methyl-3,4,5-tri-O-galloylquinic acid (GQA-16). Furthermore, through HPLC-MS analysis it was identified additional 10 galloylquinic acid derivatives: 3-Ogalloylquinic acid, 4-O-galloylquinic acid, 5-O-galloylquinic acid, 5\'-O-methyl-4-Ogalloylquinic acid, 5\'-O-methyl-5-O-galloylquinic acid, 5\'-O-methyl-3,4,5-tri-Ogalloylquinic acid, 5\'\'\'-O-methyl-3,4,5-tri-O-galloylquinic acid, 5\',5\'\'-di-O-methyl-3,4,5-tri- O-galloylquinic acid, 5\',5\'\'\'-di-O-methyl-3,4,5-tri-O-galloylquinic acid, 5\'\',5\'\'\'-di-O-methyl- 3,4,5-tri-O- galloylquinic acid. The HPLC developed method was suitable to quantify nine galloylquinic derivatives (GQA-1, GQA-5, GQA-6, GQA-7, GQA-8, GQA-9, GQA-10, GQA-15, GQA-16) and two flavonoids, quercitrin and afzelin, related to the selectivity, linearity, sensitivity, precision and accuracy parameters. Through multivariate statistical analysis, it was possible to conclude that all ten diferrent populations of C. langsdorffii cultivated displayed similar qualitative and quantitative chemical profiles among isolated months and different quantitative profiles among different months.

Submitted by Jean Medeiros (jeanletras@uepb.edu.br) on 2016-04-13T13:00:25Z No. of bitstreams: 1 PDF - Rayanne Sales de Araújo Batista.pdf: 2799391 bytes, checksum: bfd7e21254a6a5383f8798d74f80923d (MD5) / Approved for entry into archive by Secta BC (secta.csu.bc@uepb.edu.br) on 2016-06-13T20:27:28Z (GMT) No. of bitstreams: 1 PDF - Rayanne Sales de Araújo Batista.pdf: 2799391 bytes, checksum: bfd7e21254a6a5383f8798d74f80923d (MD5) / Made available in DSpace on 2016-06-13T20:28:54Z (GMT). No. of bitstreams: 1 PDF - Rayanne Sales de Araújo Batista.pdf: 2799391 bytes, checksum: bfd7e21254a6a5383f8798d74f80923d (MD5) Previous issue date: 2015-03-19 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / Retinoic acid (RA), widely used in dermatological and cosmetic products, has low stability in the presence of air and light, with sensitivity to heat and oxidation, so it is particularly important to implement the quality control of its finished products performing tests indicators of stability. Therefore, the objective was to develop an analytical method to evaluate the thermal stability of an RA cream formulation through the correlation of analytical techniques, high performance liquid chromatography with ultraviolet detection efficiency (HPLC-UV), differential scanning calorimetry (DSC) and vibrational absorption spectroscopy in the infrared Fourier transform spectroscopy (FTIR). Previously been established chromatographic conditions for development of the analytical method using HPLC-UV system, which was subjected to analytical tests specified in RE ANVISA Nº 899/2003 for validation. For evaluation of the thermal stability the cream samples were subjected to thermal stress in an oven at temperatures of 60, 70 and 80 °C and subsequently analyzed by HPLC-UV over the period of 0, 24, 48 and 72 h. DSC analyzes and FTIR spectra were carried out from the binary mixture (BM) of the RA and excipients of the cream formulation to investigate possible physical and/or chemical interactions. According to the data obtained it was possible to develop an analytical method by validated HPLC-UV, and based thereon, for analyzing and quantifying the RA content cream formulation, it has been found that from 70 ° C caused a decrease in the content of RA, and 0-order kinetics; and 80 ° C, followed a kinetic order 2 by setting up a reaction of bimolecular type. The analytical techniques DSC and FTIR showed the absence of chemical and physical interaction in most MB among the components of the formulation, except only for the carrier sodium metabisulfite. Thus, we can infer that it has a well-defined thermal behavior and compatibility of its components. / O ácido retinoico (AR), largamente utilizado em produtos dermatológicos e cosméticos, apresenta baixa estabilidade na presença de ar e luz, com sensibilidade ao calor e à oxidação, assim, é particularmente importante implementar o controle de qualidade de seus produtos acabados realizando ensaios indicadores de estabilidade. Logo, objetivou-se desenvolver um método analítico para avaliar a estabilidade térmica de uma formulação creme de AR através da correlação de técnicas analíticas, cromatografia líquida de alta eficiência com detecção ultravioleta (CLAE-UV), calorimetria exploratória diferencial (DSC) e espectroscopia vibracional de absorção na região do infravermelho com transformada de Fourier (FTIR). Previamente foram estabelecidas as condições cromatográficas para desenvolvimento do método analítico utilizando um sistema de CLAE-UV, o qual foi submetido aos testes analíticos especificados na RE ANVISA nº 899/2003 para validação do mesmo. Para avaliação da estabilidade térmica, as amostras do creme foram submetidas a estresse térmico em estufa nas temperaturas de 60, 70 e 80 º C, e posteriormente analisadas por CLAE-UV no período de 0, 24, 48 e 72 h. As análises de DSC e dos espectros de FTIR foram realizadas a partir das misturas binárias (MB) do AR e excipientes da formulação creme a fim de investigar possíveis interações físicas e/ou químicas. De acordo com os dados obtidos foi possível desenvolver um método analítico por CLAE-UV validado, e com base no mesmo, para análise e quantificação do teor de AR em formulação creme, constatou-se que a partir de 70 ° C ocorreu redução no teor de AR, e cinética de ordem 0; a 80 ° C, obedeceu uma cinética de ordem 2, configurando uma reação do tipo bimolecular. As técnicas analíticas DSC e FTIR mostraram a ausência de interação física e química na maioria das MB entre os componentes da formulação, com exceção apenas para o excipiente metabissulfito de sódio. Desta forma, podemos inferir que a mesma apresenta um comportamento térmico bem definido e compatibilidade entre seus componentes.

No description available.

Cereals are rich in phenolic acids, a group of secondary plant metabolites that are associated with reduced risk of chronic diseases. The objective was to develop and internally validate a method for extraction and quantification of phenolic acids in cereals using HPLC-UV and to apply this method for quantification of the content of phenolic acids in several species of Swedish cereals. Different procedures for extraction of phenolic acids from cereal grains using acid or base hydrolysis with and without subsequent enzymatic treatment were tested. Both the extraction procedure and the chromatographic conditions for quantification with HPLC-UV were optimized. Phenolic acids from 14 cereal samples, representing different cultivars of rye, wheat, barley, and oat, were extracted and analyzed under optimized conditions. Using the optimized method, 15 phenolic acids could be quantified with limits of detection and quantification ranging from 0.4 to 11.4 µg/g and from 1.3 to 38.0 µg/g, respectively. The hydrolysis procedure and further sample treatment showed a substantial effect on the yield of phenolic acids from cereals. The highest yield was achieved by 90‑minute base hydrolysis at room temperature using sodium hydroxide solution containing ascorbic acid and EDTA. Mean recoveries ranged from 88 to 108%. The following phenolic acids were found in the analyzed cereal grains with ferulic acid being the most abundant one: p‑hydroxybenzoic acid, vanillic acid, vanillin, caffeic acid, syringic acid, ferulic acid, sinapic acid, and 3,4‑dihydroxybenzaldehyde. A further compound was p‑coumaric acid or the co‑eluting syringaldehyde or a mixture of both. The content of phenolic acids in Swedish cereals ranged from 6 µmol/g DM in rye to 3 µmol/g DM in oat and a barley cultivar. In conclusion, a simple and accurate method for extraction and quantification of phenolic acids in cereals was developed and successfully applied. / Getreide ist reich an Phenolsäuren, einer Gruppe pflanzlicher Sekundärmetabolite, die mit einem verringerten Risiko für chronische Erkrankungen in Verbindung gebracht wird. Ziel war es, eine Methode zur Phenolsäure-Extraktion aus Getreide und Quantifizierung mittels HPLC-UV zu entwickeln, intern zu validieren und diese im Anschluss anzuwenden, um den Phenolsäure-Gehalt in mehreren schwedischen Getreidearten zu quantifizieren. Verschiedene Verfahren zur Phenolsäure-Extraktion aus Getreide unter Verwendung von Säure- oder Basenhydrolyse mit oder ohne nachfolgender enzymatischer Hydrolyse wurden getestet. Es wurden sowohl das Extraktionsverfahren als auch die chromatographischen Bedingungen zur Quantifizierung mittels HPLC-UV optimiert. Phenolsäuren von 14 Getreideproben, darunter Kultivare von Roggen, Weizen, Gerste und Hafer, wurden unter optimierten Bedingungen extrahiert und analysiert. Mit der optimierten Methode konnten 15 Phenolsäuren mit Nachweisgrenzen von 0,4 bis 11,4 µg/g und Bestimmungsgrenzen von 1,3 bis 38,0 µg/g quantifiziert werden. Hydrolyseverfahren und weitere Probenbehandlung haben die Phenolsäure-Ausbeute von Getreide wesentlich beeinflusst. Die höchste Ausbeute wurde durch eine 90‑minütige Basenhydrolyse bei Raumtemperatur unter Verwendung von Natronlauge mit Ascorbinsäure und EDTA erzielt. Die mittlere Wiederfindung betrug 88 bis 108%. In den untersuchten Getreideproben wurden folgende Phenolsäuren gefunden mit Ferulasäure als häufigster Verbindung: p-Hydroxybenzoesäure, Vanillinsäure, Vanillin, Kaffeesäure, Syringasäure, Ferulasäure, Sinapinsäure und 3,4‑Dihydroxybenzaldehyd. Eine weitere Verbindung war p‑Cumarsäure oder der co‑eluierende Syringaldehyd oder eine Mischung aus beiden. Der Phenolsäure-Gehalt reichte von 6 µmol/g DM in Roggen bis 3 µmol/g DM in Hafer und einem Gerstenkultivar. Zusammenfassend wurde eine einfache und genaue Methode zur Phenolsäure-Extraktion und Quantifizierung in Getreide entwickelt und erfolgreich angewendet.

<p>The objective of this master thesis was to develop an analytical method for the quantification of the cancer drug Imatinib and its main metabolite CGP74588 in plasma. Imatinib is used in the treatment of chronic myeloid leukemia and gastrointestinal stroma tumors. A quantitative analytical method was developed where reversed-phase columns with different stationary phases were studied and the sensitivity was tested with both UV detectors and a mass spectrometric detection. Since the substances were measured in plasma a solid-phase extraction was developed to purify the samples before analysis. The column chosen for the separation was the Max-RP C12 column (100 x 3 mm, 4 μm particle size) manufactured by Phenomenex with a gradient mobile phase with 1% formic acid in methanol and water. The gradient was as follows; 0 min 15:85, 7 min 60:40, 9 min 60:40 with a total runtime of 13.5 min. The internal standard chosen was Opipramol. Mass spectrometric detection using a sonic spray ionization interface in positive mode proved to be about as sensitive as UV detection at 261 nm. The generated (M+H+)+ ions were isolated and fragmented with the use of three mass spectrometric methods; one for Imatinib (transition 494 —› 394), one for CGP74588 (transition 480 —› 394) and one for Opipramol (transition 364 —› 171). For the purification of the plasma samples an Oasis HLB solid-phase extraction cartridge was selected and the recoveries were close to 100%.</p><p>The developed method was partially validated and showed coefficients of variation (CV) for intra-and inter-day precision between 0.4 and 5.4% with UV detection. The validation results for the mass spectrometer were inconclusive.</p>

The objective of this master thesis was to develop an analytical method for the quantification of the cancer drug Imatinib and its main metabolite CGP74588 in plasma. Imatinib is used in the treatment of chronic myeloid leukemia and gastrointestinal stroma tumors. A quantitative analytical method was developed where reversed-phase columns with different stationary phases were studied and the sensitivity was tested with both UV detectors and a mass spectrometric detection. Since the substances were measured in plasma a solid-phase extraction was developed to purify the samples before analysis. The column chosen for the separation was the Max-RP C12 column (100 x 3 mm, 4 μm particle size) manufactured by Phenomenex with a gradient mobile phase with 1% formic acid in methanol and water. The gradient was as follows; 0 min 15:85, 7 min 60:40, 9 min 60:40 with a total runtime of 13.5 min. The internal standard chosen was Opipramol. Mass spectrometric detection using a sonic spray ionization interface in positive mode proved to be about as sensitive as UV detection at 261 nm. The generated (M+H+)+ ions were isolated and fragmented with the use of three mass spectrometric methods; one for Imatinib (transition 494 —› 394), one for CGP74588 (transition 480 —› 394) and one for Opipramol (transition 364 —› 171). For the purification of the plasma samples an Oasis HLB solid-phase extraction cartridge was selected and the recoveries were close to 100%. The developed method was partially validated and showed coefficients of variation (CV) for intra-and inter-day precision between 0.4 and 5.4% with UV detection. The validation results for the mass spectrometer were inconclusive.

Dietary food supplements are among the most rapidly growing sectors in the food product industry. The majority of consumers trust in the safety and efficacy of these products. For these reasons is a quality control required and analytical methodologies for this must be used. For identification and quantitative analysis four flavonoids diosmin, hesperidin, rutin and troxerutin in food supplements was used HPLC/MS method. For identification and quantitative analysis three carotenoids betacarotene, lutein and zeaxanthin in food supplements was used HPLC/UV/ViS/DAD method. Separation of flavonoids was achieved on the column ZORBAX POROSHELL 120 EC-C18 (50 x 4,6 mm, 2,7 um) and separation of carotenoids on the column ZORBAX SB CN (75 x 4,6 mm, 3,5 um). The amount of flavonoids and carotenoids in tablets and capsules was determined altogether in 12 different commercial preparations.

Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2016-09-06T15:39:12Z No. of bitstreams: 1 Tese Adalberto Menezes Filho 26.03.2010.pdf: 4529406 bytes, checksum: 23a6a27845c477df8cc06bee3255777f (MD5) / Approved for entry into archive by Vanessa Reis (vanessa.jamile@ufba.br) on 2016-09-08T10:44:55Z (GMT) No. of bitstreams: 1 Tese Adalberto Menezes Filho 26.03.2010.pdf: 4529406 bytes, checksum: 23a6a27845c477df8cc06bee3255777f (MD5) / Made available in DSpace on 2016-09-08T10:44:55Z (GMT). No. of bitstreams: 1 Tese Adalberto Menezes Filho 26.03.2010.pdf: 4529406 bytes, checksum: 23a6a27845c477df8cc06bee3255777f (MD5) / CNPq / Foram desenvolvidas, validadas e aplicadas duas metodologias analíticas por SPME e análise por GC-MS e HPLC-UV-Vis, para determinar resíduos de agrotóxicos em manga. 14 compostos foram analisados por GC-MS (clofentezina, carbofuran, diazinon, parationa, malationa, fentiona, tiabendazol, imazalil, bifentrina, permetrina, procloraz, piraclostrobina, difenoconazol, azoxistrobina) e 10 por HPLC-UV-Vis (tiabendazol, carbofuran, azoxistrobina, procloraz, fentiona, clofentezina, permetrina, abamectina, carbosulfan e bifentrina). Diferentes parâmetros que influenciam na eficiência da extração foram avaliados (Tipo de fibra, modo de extração, temperatura e tempo de extração e dessorção, velocidade de agitação e força iônica). Os melhores resultados foram obtidos com fibra de PA e DI a 50°C por 30 min, com agitação a 250 rpm e dessorção por 5 min a 280°C no GC- MS e no modo estático por 15 min na interface SPME-HPLC. Na validação foram avaliados o efeito da matriz, a linearidade das curvas analíticas, LOD, LOQ, precisão e exatidão. O método por SPME-GC-MS apresentou linearidade entre 3,3 e 1665,0 µg kg-1, LOD entre 1,0 e 3,3 µg kg-1 e LOQ entre 3,3 e 33,3 µg kg-1. O método por SPME-HPLC- UV-Vis apresentou linearidade entre 2,0 e 250,0 µg kg-1, LOD entre 0,6 e 3,3 µg kg-1 e LOQ entre 2,0 e 10,0 µg kg-1. Nos dois métodos foram obtidos CV menores que 20%. Os métodos foram aplicados na análise de amostras coletadas em Salvador-BA e Aracaju-SE. Nas amostras de Salvador foram detectados resíduos de sete compostos e nas de Aracaju resíduos de cinco compostos. Entretanto, as concentrações estavam abaixo dos valores estabelecidos pela Legislação Brasileira. / Were developed, validated and applied two analytical methodologies by SPME and GC-MS and HPLC-UV-Vis analysis to determine pesticide residues in mango. 14 compounds were analyzed by GC-MS (clofentezine, carbofuran, diazinon, methyl parathion, malathion, fenthion, thiabendazole, imazalil, bifenthrin, permethrin, prochloraz, pyraclostrobin, difenoconazole, azoxystrobin) and 10 for HPLC-UV-Vis (thiabendazole, carbofuran, azoxystrobin, prochloraz, fenthion, clofentezine, permethrin, abamectin, bifenthrin and carbosulfan). Different parameters influencing the extraction efficiency were evaluated (fiber type, extraction mode, temperature, extraction and desorption times, stirring velocities and ionic strength. The best results were obtained using PA fiber and DI mode at 50°C form 30 min, along with stirring at 250rpm and desorption for 5 min at 280°C in the GC-MS and estatic mode for 15 min in the SPME-HPLC interface. For validation, we assessed the matrix effect, the linearity of calibration curves, LOD, LOQ, precision and accuracy. The method for SPME-GC-MS showed linearity between 3.3 and 1665.0 mg kg- 1, LOD between 1.0 and 3.3 µg kg-1 and LOQ between 3.3 and 33.3 µg kg-1. The method for SPME-HPLC-UV-Vis showed linearity between 2.0 and 250.0 µg kg-1, LOD between 0.6 and 3.3 µg kg-1 and LOQ between 2.0 and 10.0 µg kg-1. In both methods were obtained CV below 20%. The methods were applied in the analysis of samples collected in Salvador- BA and Aracaju-SE. In samples from Salvador seven compounds residues were detected and in samples from Aracaju five compounds residues were detected. However, the concentrations were below the values established by Brazilian legislation