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Evolution of ethyl carbamate during Madeira wine ageing by GC-MS: a new methodology

Leça, João Micael da Silva
Fonte: Universidade da Madeira Publicador: Universidade da Madeira
Tipo: Dissertação de Mestrado
Publicado em /11/2014 ENG
Relevância na Pesquisa
96.33%
Recently, ethyl carbamate (EC) was reclassified by the International Agency for Research on Cancer (IARC) as "probably carcinogenic to humans" and occurs mainly in fermented beverages. Nowadays many countries have set limit values for EC in alcoholic beverages. In this sense and taking into account the low concentrations found in alcoholic beverages, the scientific community has shown interest for the development of new analytical methods, whereby its simplification plays an important role in the EC control and prevention. Firstly, a simple, rapid and sensitive methodology was developed for the EC quantification in fortified wines by microextraction by packed sorbent (MEPS) with gas chromatography coupled with a mass spectrometer detector (GC-MS). This method showed good linearity (R2 = 0.999) and sensitivity (LOD = 1.5 μg/L). The accuracy of the method was assessed by means of repeatability and reproducibility (RSD < 7%). Moreover, a good recovery has been demonstrated (97 – 106%) as well as its applicability (16 fortified wines). Thus, the developed methodology has proven to be an excellent approach for routine quantification of EC in fortified wines. The EC evolution was also evaluated during a year and half of Madeira wine ageing submitted to two traditional ageing methods...

Microextraction in packed sorbent for determination of sulfonamides in egg samples by liquid chromatography and spectrophotometric detection

SALAMI, Fernanda H; QUEIROZ, Maria Eugênia C
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
56.31%
The present work describes a successful application of microextraction packed sorbent and liquid chromatography with diode array detection (MEPS/LC-DAD) for simultaneous determination of the sulfonamides (sulfacetamide, sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxypiridazine and sulfamethoxazole) in egg samples. The MEPS variables (pH of the sample, draw-eject cycles, ionic strength, and desorption procedure) were optimized, in order to improve the sensitivity of the proposed method. The method was shown to be linear at concentrations ranging from 30 ng g-1 (limit of quantification, LOQ) to 300 ng g-1. This LOQ value is lower than those established as the maximum residue limit (MRL) for egg samples (100 µg kg-1). The accuracy values were adequate for all analytes (> 94%), as well as the inter-day precision data, with coefficient of variation lower than 10%. On the basis of analytical validation, the MEPS/LC methodology has been shown to be a promising alternative for analysis of sulfonamides in egg samples.; O presente trabalho descreve a aplicação bem sucedida da microextração em sorvente empacotado e cromatografia líquida com detecção de arranjo de diodos (MEPS/LC-DAD) para a determinação simultânea das sulfonamidas (sulfacetamida...

Microextraction in packed sorbent for analysis of antidepressants in human plasma by liquid chromatography and spectrophotometric detection

CHAVES, Andrea R.; LEANDRO, Fernanda Z.; CARRIS, Juciene A.; QUEIROZ, Maria Eugenia C.
Fonte: ELSEVIER SCIENCE BV Publicador: ELSEVIER SCIENCE BV
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
86.54%
A sensitive and reproducible method by microextraction packed sorbent and liquid chromatography with UV detection (MEPS/LC-UV) is described for the determination of new generation antidepressants (sertraline, mirtazapine, fluoxetine, citalopram and paroxetine) in human plasma samples. The MEPS variables, such as sample volume, pH, number of extraction cycles (draw-eject), and desorption conditions (solvent and solvent volume of elution) influenced the MEPS/LC efficiency significantly. Important factors in the optimization of MEPS efficiency, as well as washing steps and carryover effect are discussed. The analyses were carried out using small sample volumes (400 mu L.), and in a short time period (3 min for the entire sample preparation step). The MEPS/LC-UV method was shown to be linear at concentrations ranging from the limit of quantification (LOQ) to 1000 ng mL(-1). The LOQ values ranged from 10 to 25 ng mL(-1). The inter-day precision of the method presented coefficient of the variation ranging from 1.3% to 8.7%. On the basis of analytical validation, it is shown that the MEPS/LC-UV methodology is adequate for antidepressant analysis, from therapeutic to toxic levels. In order to evaluate the proposed method for clinical use, the MEPS/LC-UV method was applied to analysis of plasma samples from elderly depressed patients. (C) 2010 Elsevier B.V. All rights reserved.; Fundacao de Amparo a Pesquisa do Estado de Sao Paulo (FAPESP); Conselho Nacional de Desenvolvimento Cientifico e Tecnologico (CNPq)

Desenvolvimento das barras imunosorventes de agitação e avaliação das técnicas extração sortiva em barra de agitação, microextração em sorvente empacotado e cromatografia líquida para análise de antidepressivos em amostras de plasma; Development of immunosorbent stir bars and evaluation of stir bar sorptive extraction, microextraction by packed sorbent and liquid chromatography for the analysis of antidepressants in plasma samples

Leandro, Fernanda Zampieri
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 15/12/2010 PT
Relevância na Pesquisa
126.55%
Neste trabalho, os anticorpos policlonais e monoclonais anti-fluoxetina foram produzidos em coelhos e camundongos, respectivamente, por imunização com o conjugado fluoxetina-soroalbumina bovina. Os anticorpos obtidos foram caracterizados em função da especificidade contra o fármaco por ELISA (enzyme linked immunosorbent assay) e posteriormente, purificados por afinidade em coluna fluoxetina-agarose labmade. Os anticorpos purificados foram imobilizados covalentemente na superfície vítrea das barras SBSE (extração sortiva em barra de agitação) labmade. Após a derivatização das barras com 3-aminopropiltrietoxisilano, dois métodos distintos de acoplamento dos anticorpos às barras SBSE foram avaliados: ativação com glutaraldeído e succinilação seguida de ativação via éster N-hidroxisuccinimida (NHS). A funcionalização das barras SBSE foi comprovada através da imobilização de enzima peroxidase (HRP) em lugar do anticorpo e posterior ensaio enzimático com as barras. Várias barras SBSE com diferentes áreas (1,2; 2,4; e 4,0 cm2) foram preparadas, dentre as quais, as com maior área imunosorvente apresentaram maiores taxas de recuperação do fármaco. A avaliação da morfologia da superfície da barra SBSE imunosorvente foi realizada através de Microscopia Eletrônica de Varredura (MEV). As variáveis do processo SBSE de imunoafinidade foram otimizadas para estabelecer o equilíbrio de sorção antígeno-anticorpo em um menor tempo de análise e obtenção de limite de quantificação compatível com o intervalo terapêutico do fármaco. As capacidades adsortivas das barras imunosorventes foram de 1...

Avaliação das técnicas de microextração e eletroforese capilar em meio não aquoso (NACE) para determinação de antidepressivos em amostras de plasma para fins de monitorização terapêutica; Evaluation of microextractions techniques and nonaqueous capillary electrophoresis (NACE) for the determination of antidepressants in plasma samples for therapeutic drug monitoring

Catai, Ana Paula Formenton
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 02/03/2012 PT
Relevância na Pesquisa
56.22%
A monitorização terapêutica tem sido descrita como um recurso clínico valioso, na individualização do regime de dosagem, de acordo com a concentração do fármaco em amostras de plasma ou soro. O objetivo da monitorização terapêutica é assegurar a eficácia clínica e minimizar os efeitos adversos dos fármacos prescritos na clínica. A química analítica moderna tem sido direcionada para a simplificação dos métodos através da miniaturização dos sistemas analíticos, minimização do consumo de solvente orgânico e do volume da amostra. Neste contexto, metodologias analíticas utilizando as técnicas de microextração, extração sortiva em barra de agitação (SBSE) e microextração em sorvente empacotado (MEPS), juntamente com a eletroforese capilar em solução não-aquosa (NACE) foram desenvolvidas para fins monitorização terapêutica de antidepressivos inibidores seletivos da recaptação de serotonina (ISRSs: fluoxetina, sertralina, paroxetina e citalopram) em amostras de plasma de pacientes em terapia com ISRSs. Inicialmente foram padronizadas as condições eletroforéticas com detecção espectrofotométrica (UV) para análise simultânea dos ISRSs em amostras de plasma. Dentre as condições avaliadas (diferentes soluções de eletrólitos em meio aquoso e não aquoso...

Análise de estatinas em plasma humano utilizando microextração por dispositivo preenchido com sorvente (MEPS) e cromatografia líquida acoplada à espectrometria de massas sequencial (LC-MS/MS); Determination of statins in human plasma using microextraction in packed syringe (MEPS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS)

Ortega, Scarlet Nere
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 20/09/2013 PT
Relevância na Pesquisa
66.37%
As elevadas taxas de colesterol plasmático representam um grande risco à saúde, uma vez que podem causar doenças cardiovasculares. Para o tratamento e prevenção da dislipidemia são utilizados medicamentos reguladores do colesterol, como as estatinas. Embora eficazes e extensamente utilizados, esses fármacos apresentam efeitos adversos se administrados na dosagem errada. Assim, faz-se necessário o desenvolvimento de um método de monitorização terapêutica a fim de se ajustar a concentração desses compostos no sangue. Este trabalho visa o desenvolvimento de um método para análise de pravastatina (PRA), atorvastatina (AT), fluvastatina (FLV) e sinvastatina (SV) em plasma humano usando cromatografia líquida acoplada à espectrometria de massas (LC-MS). Na etapa de preparo de amostras, de forma inédita, utilizou-se a técnica microextração por sorvente empacotado (MEPS) para a análise de plasma humano contendo quatro estatinas. Para a otimização das condições de extração avaliaram-se, por experimentos univariados, parâmetros como fase extratora, composição do solvente de eluição e de lavagem. Outros fatores como volume de amostra, ciclos de amostragem, ciclos de eluição e etapas de eluição foram avaliados empregando-se planejamento experimental multivariado. A extração foi realizada utilizando-se uma fase estacionária C18 Chromabond como sorvente. O método MEPS-LC-MS/MS desenvolvido foi validado baseando-se nas recomendações da agência nacional de vigilância sanitária (ANVISA) e apresentou linearidade...

Avaliação do emprego da técnica MEPS na análise de agrotóxicos em caldo de cana-de-açúcar por GC-MS; Evaluation of MEPS technique applied in pesticides analysis in sugarcane juice by GC-MS

Fumes, Bruno Henrique
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 12/02/2015 PT
Relevância na Pesquisa
56.58%
O uso de técnicas miniaturizadas de preparo de amostra vem se tornando uma tendência cada vez mais crescente em química analítica. Dentre elas o MEPS (Microextraction by a Packed Sorbent) apresenta grande potencial por poder ser acoplado on-line, sem grandes modificações, à cromatografia gasosa e líquida, não necessitando de grande quantidade de tempo para análise e seu cartucho sorvente ser reutilizável. O uso de MEPS, foi mais explorado até o presente momento na análise de fármacos em fluídos biológicos; dessa forma existe um pequeno número de publicações que exploram o uso dessa técnica na determinação de agrotóxicos em matrizes de alimentos. Por esse motivo, o presente trabalho teve como objetivo a avaliação do uso dessa técnica na determinação de seis agrotóxicos utilizados no cultivo da cana-de-açúcar (tebutiurom, carbofurano, atrazina, metribuzim, ametrina e bifentrina) em amostras de garapa. Para o desenvolvimento desse estudo foram verificadas dentre as variáveis pH, força iônica, solvente de eluição e volume do solvente de eluição, quais poderiam afetar o desempenho da técnica em diferentes fases extratoras, empregando nessa etapa de otimização planejamento fatorial fracionário 24-1. As fases avaliadas foram C18 Chromabond e HLB Oasis...

Desenvolvimento de métodos miniaturizados de extração em fase sólida para a pré-concentração de produtos de degradação de fluoroquinolonas e sulfonamidas em matrizes aquosas; Development of methods for miniaturized solid phase extraction for preconcentration of degradation products of fluoroquinolones and sulfonamides in aqueous matrix

Martins, Júlia
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 10/03/2015 PT
Relevância na Pesquisa
46.11%
A presença de antibióticos em águas superficiais e subterrâneas é motivo de preocupação, devido ao surgimento de bactérias resistentes. Contudo, a maioria dos trabalhos publicados na literatura científica mantém o foco nos antibióticos inalterados, sendo que as moléculas degradadas também estão no ambiente. Esses produtos de degradação podem ser tão ou mais prejudiciais do que as moléculas que lhes deram origem. Esse trabalho teve por objetivo desenvolver métodos de extração utilizando a microextração por sorvente empacotado (MEPS) para pré-concentrar e recuperar produtos de fotodegradação de representantes das sulfonamidas (sulfametazina) e fluoroquinlonas (ciprofloxacino), duas das mais importantes classes de antibióticos. MEPS é considerada uma técnica promissora utilizando pequenos volumes de amostra e de solventes, além de empregar pequenas quantidades de fase extratora, que ainda pode ser reutilizada. Foram comparadas as fases Oasis® HLB e nanotubos de carbono, sendo que a primeira apresentou melhores resultados. Seis produtos de degradação da sulfametazina (SMZ) e oito produtos do ciprofloxacino (CIP)...

Microextraction in packed sorbent for determination of sulfonamides in egg samples by liquid chromatography and spectrophotometric detection

Salami,Fernanda H; Queiroz,Maria Eugênia C
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/09/2011 EN
Relevância na Pesquisa
56.31%
The present work describes a successful application of microextraction packed sorbent and liquid chromatography with diode array detection (MEPS/LC-DAD) for simultaneous determination of the sulfonamides (sulfacetamide, sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxypiridazine and sulfamethoxazole) in egg samples. The MEPS variables (pH of the sample, draw-eject cycles, ionic strength, and desorption procedure) were optimized, in order to improve the sensitivity of the proposed method. The method was shown to be linear at concentrations ranging from 30 ng g-1 (limit of quantification, LOQ) to 300 ng g-1. This LOQ value is lower than those established as the maximum residue limit (MRL) for egg samples (100 µg kg-1). The accuracy values were adequate for all analytes (> 94%), as well as the inter-day precision data, with coefficient of variation lower than 10%. On the basis of analytical validation, the MEPS/LC methodology has been shown to be a promising alternative for analysis of sulfonamides in egg samples.

Assessing stir bar sorptive extraction and microextraction by packed sorbent for determination of selective serotonin reuptake inhibitor antidepressants in plasma sample by non-aqueous capillary electrophoresis

Catai,Ana Paula F.; Picheli,Flávio P.; Carrilho,Emanuel; Queiroz,Maria Eugênia C.
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/10/2013 EN
Relevância na Pesquisa
126.51%
Two approaches based on partition equilibrium, stir bar sorptive extraction (SBSE) and microextraction by packed sorbent (MEPS) were evaluated for determination of selective serotonin reuptake inhibitor antidepressants (SSRI): fluoxetine, sertraline, citalopram and paroxetine in plasma sample by non-aqueous capillary electrophoresis (NACE) with spectrophotometric detection. The SBSE/NACE and MEPS/NACE methods showed linear range from the LOQ up to 500 ng mL-1. LOQ values ranged from 10 to 30 ng mL(-1)1 in both techniques, depending on the compound. The inter-assay precision of the methods presented coefficient of variation lower than 12%. According to the analytical validation results, the methods are adequate for SSRI antidepressant analyses at therapeutic levels, consequently, amenable to therapeutic drug monitoring. These methods reduced the volumes of biological samples, the use of organic solvents and the number of steps involved in sample preparation.

Application of microextraction by packed sorbent to isolation of psychotropic drugs from human serum

Wietecha-Posłuszny, Renata; Garbacik, Aneta; Woźniakiewicz, Michał; Moos, Agnieszka; Wieczorek, Marcin; Kościelniak, Paweł
Fonte: Springer-Verlag Publicador: Springer-Verlag
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
86.55%
A method of microextraction by packed sorbent (MEPS) followed by liquid chromatography with diode array detection has been developed and optimized for the extraction of six tricyclic antidepressants (amitriptyline, nortriptyline, imipramine, desipramine, doxepin, nordoxepin) from human serum. The optimal parameters of MEPS extraction (type of sorbent, volume of sample, composition, and volume of washing and elution solutions) for these drugs in spiked samples were defined. The developed MEPS procedure was validated and then successfully applied to the analysis of serum reference material. The limit of detection (0.02–0.05 μg/mL), intraday (2.7–8.8%) and interday (4.4–11.6%) precision (RSD), and the accuracy of the assay (94.5–108.8%) at three concentration levels—0.2, 0.5, and 0.8 μg/mL—were estimated. The accuracy of the method was evaluated by the analysis of certified reference material. Moreover, the validated procedure was compared with the solid-phase extraction technique. Finally, microextraction by packed sorbent was assessed as a suitable tool in forensic and clinical methods for serum sample preparations.

A Micro-Extraction Technique Using a New Digitally Controlled Syringe Combined with UHPLC for Assessment of Urinary Biomarkers of Oxidatively Damaged DNA

Mendes, Berta; Silva, Pedro; Aveiro, Fernando; Pereira, Jorge; Câmara, José S.
Fonte: Public Library of Science Publicador: Public Library of Science
Tipo: Artigo de Revista Científica
Publicado em 06/03/2013 EN
Relevância na Pesquisa
46.1%
The formation of reactive oxygen species (ROS) within cells causes damage to biomolecules, including membrane lipids, DNA, proteins and sugars. An important type of oxidative damage is DNA base hydroxylation which leads to the formation of 8-oxo-7,8-dihydro-2′-deoxyguanosine (8-oxodG) and 5-hydroxymethyluracil (5-HMUra). Measurement of these biomarkers in urine is challenging, due to the low levels of the analytes and the matrix complexity. In order to simultaneously quantify 8-oxodG and 5-HMUra in human urine, a new, reliable and powerful strategy was optimised and validated. It is based on a semi-automatic microextraction by packed sorbent (MEPS) technique, using a new digitally controlled syringe (eVol®), to enhance the extraction efficiency of the target metabolites, followed by a fast and sensitive ultrahigh pressure liquid chromatography (UHPLC). The optimal methodological conditions involve loading of 250 µL urine sample (1∶10 dilution) through a C8 sorbent in a MEPS syringe placed in the semi-automatic eVol® syringe followed by elution using 90 µL of 20% methanol in 0.01% formic acid solution. The obtained extract is directly analysed in the UHPLC system using a binary mobile phase composed of aqueous 0.1% formic acid and methanol in the isocratic elution mode (3.5 min total analysis time). The method was validated in terms of selectivity...

Quantitative Analysis of Cepharanthine in Plasma Based on Semiautomatic Microextraction by Packed Sorbent Combined with Liquid Chromatography

Desgrouas, Camille; Desbordes, Marc; Dormoi, Jérôme; Ollivier, Evelyne; Parzy, Daniel; Taudon, Nicolas
Fonte: Hindawi Publishing Corporation Publicador: Hindawi Publishing Corporation
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
86.38%
The spread of Plasmodium falciparum resistance toward most of the used drugs requires new antimalarial compounds. Taking advantage of the biodiversity, the ethnopharmacological approach opens the way for the discovery and the characterization of potent original molecules. Previous works led to the selection of a bisbenzylisoquinoline, cepharanthine, extracted from Stephania rotunda, which is mainly present in Cambodia. A sensitive and selective liquid chromatography method has been developed for the determination of cepharanthine in mouse plasma. The method involved a semiautomated microextraction by packed sorbent (MEPS) using 4 mg of solid phase silica-C8 sorbent. LC separation was performed on a Kinetex XB-C18 column (2.6 µm) with a mobile phase of acetonitrile containing formic acid and 10 mM ammonium formate buffer pH 3.5. Data were acquired at 282 nm with a diode array detector. The drug/internal standard peak area ratios were linked via linear relationships to plasma concentrations (75–2,000 ng/mL). Precision was below 5% and accuracy was 99.0–102%. Extraction recovery of cepharanthine was 56–58%. The method was successfully used to determine the pharmacokinetic profile of cepharanthine in healthy and Plasmodium berghei infected mice. The infection did not impact pharmacokinetic parameters of cepharanthine.

Microextraction by Packed Sorbent (MEPS) and Solid-Phase Microextraction (SPME) as Sample Preparation Procedures for the Metabolomic Profiling of Urine

Silva, Catarina; Cavaco, Carina; Perestrelo, Rosa; Pereira, Jorge; Câmara, José S.
Fonte: MDPI Publicador: MDPI
Tipo: Artigo de Revista Científica
Publicado em 27/01/2014 EN
Relevância na Pesquisa
86.46%
For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS) and solid-phase microextraction (SPME), completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones.

Rapid and sensitive methodology for determination of ethyl carbamate in fortified wines using microextraction by packed sorbent and gas chromatography with mass spectrometric detection

Leça, João M.; Pereira, Vanda; Pereira, Ana C.; Marques, José C.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
126.57%
This work presents a new methodology to quantify ethyl carbamate (EC) in fortified wines. The presented approach combines the microextraction by packed sorbent (MEPS), using a hand-held automated analytical syringe, with one-dimensional gas chromatography coupled with mass spectrometry detection (GC–MS). The performance of different MEPS sorbent materials was tested, namely SIL, C2, C8, C18, and M1. Also, several extraction solvents and the matrix effect were evaluated. Experimental data showed that C8 and dichloromethane were the best sorbent/solvent pair to extract EC. Concerning solvent and sample volumes optimization used in MEPS extraction an experimental design (DoE) was carried out. The best extraction yield was achieved passing 300 μL of sample and 100 μL of dichloromethane. The method validation was performed using a matrix-matched calibration using both sweet and dry fortified wines, to minimize the matrix effect. The proposed methodology presented good linearity (R2 = 0.9999) and high sensitivity, with quite low limits of detection (LOD) and quantification (LOQ), 1.5 μg L−1 and 4.5 μg L−1, respectively. The recoveries varied between 97% and 106%, while the method precision (repeatability and reproducibility) was lower than 7%. The applicability of the methodology was confirmed through the analysis of 16 fortified wines...

Desenvolvimento de fases monolíticas de sílica híbrida para microextração em sorvente empacotado (MEPS) de fármacos em amostras de plasma e análise por cromatografia líquida acoplada a espectrometria de massas em tandem (LC-MS/MS); Synthesis of hybrid silica monoliths for microextraction by packed sorbent (MEPS) to determine drugs from plasma samples by liquid chromatography-tandem mass (LC-MS/MS)

Souza, Israel Donizéti de
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 27/07/2015 PT
Relevância na Pesquisa
126.51%
Segundo a Organização Mundial da Saúde (OMS), a esquizofrenia é reconhecida como um transtorno neuropsiquiátrico grave que afeta mais de 21 milhões de pessoas em todo o mundo. Para diminuir os sintomas associados a esta doença, a maioria dos pacientes esquizofrênicos fazem uso concomitantemente de antipsicóticos, antidepressivos, ansiolíticos e anticonvulsivantes. O desenvolvimento de métodos analíticos para a determinação desses fármacos em fluidos biológicos é importante para ajustar as doses administradas, minimizar os efeitos adversos e verificar a anuência do paciente à terapia. A química analítica moderna tem se direcionado para a simplificação, através da miniaturização dos sistemas analíticos. Neste contexto, pode-se destacar a técnica de microextração em sorvente empacotado (MEPS). O desenvolvimento de novas fases extratoras para MEPS, como, os monolitos de sílica híbrida permitem pré-concentração seletiva dos analitos. Neste projeto monolitos de sílica híbrida funcionalizados com grupos aminopropil ou cianopropil foram sintetizados pelo processo sol-gel. Estes monolitos apresentaram estrutura contínua, uniforme e porosa, como evidenciado pelas imagens de microscopia eletrônica de varredura (MEV). As análises de espectroscopia vibracional na região do infravermelho por transformada de Fourier (FTIR) dos monolitos de sílica híbrida exibiram picos facilmente identificáveis...

New method for determination of (E)resveratrol in wine based on microextraction using packed sorbent and ultra-performance liquid chromatography

Gonçalves, João; Câmara, José S.
Fonte: Wiley-VCH Publicador: Wiley-VCH
Tipo: Artigo de Revista Científica
Publicado em /06/2011 ENG
Relevância na Pesquisa
116.57%
An ultra-fast and improved analytical methodology based on microextraction by packed sorbent (MEPS) combined with ultra-performance LC (UPLC) was developed and validated for determination of (E)-resveratrol in wines. Important factors affecting the performance of MEPS such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles, and sample volume were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (50–250mL) in one extraction cycle (extract–discard) and in a short time period (about 3 min for the entire sample preparation step). (E)-Resveratrol was eluted by 1 250mL of the mixture containing 95% methanol and 5% water, and the separation was carried out on a highstrength silica HSS T3 analytical column (100 mm 2.1 mm, 1.8mm particle size) using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and methanol (eluent B) in the gradient elution mode (10 min of total analysis). The method was fully validated in terms of linearity, detection (LOD) and quantification (LOQ) limits, extraction yield, accuracy, and inter/intra-day precision, using a Madeira wine sample (ET) spiked with (E)-resveratrol at concentration levels ranging from 5 to 60mg/mL. Validation experiments revealed very good recovery rate of 9575.8% RSD...

A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines

Silva, Catarina L.; Gonçalves, João L.; Câmara, José S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /08/2012 ENG
Relevância na Pesquisa
126.59%
A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). Under optimized conditions, excellent linearity View the MathML source(Rvalues2>0.9963), limits of detection of 0.006 μg mL−1 (quercetin) to 0.013 μg mL−1 (myricetin) and precision within 0.5–3.1% were observed for the target flavonols. The average recoveries of myricetin...

Development of a novel microextraction by packed sorbent-based approach followed by ultrahigh pressure liquid chromatography as a powerful technique for quantification phenolic constituents of biological interest in wines

Gonçalves, João; Mendes, Berta; Silva, Catarina L.; Câmara, José S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /03/2012 ENG
Relevância na Pesquisa
126.58%
A novel analytical approach, based on a miniaturized extraction technique, the microextraction by packed sorbent (MEPS), followed by ultrahigh pressure liquid chromatography (UHPLC) separation combined with a photodiode array (PDA) detection, has been developed and validated for the quantitative determination of sixteen biologically active phenolic constituents of wine. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (linearity, sensitivity, selectivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters on the MEPS performance such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). The wine bioactive phenolics were eluted by 250 μL of the mixture containing 95% methanol and 5% water, and the separation was carried out on a HSS T3 analytical column (100 mm × 2.1 mm, 1.8 μm particle size) using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and methanol (eluent B) in the gradient elution mode (10 min of total analysis). The method gave satisfactory results in terms of linearity with r2-values > 0.9986 within the established concentration range. The LOD varied from 85 ng mL−1 (ferulic acid) to 0.32 μg mL−1 ((+)-catechin)...

Effectiveness of high-throughput miniaturized sorbent- and solid phase microextraction techniques combined with gas chromatography–mass spectrometry analysis for a rapid screening of volatile and semi-volatile composition of wines: a comparative study

Mendes, Berta; Gonçalves, João; Câmara, José S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /01/2012 ENG
Relevância na Pesquisa
86.57%
In this study the feasibility of different extraction procedures was evaluated in order to test their potential for the extraction of the volatile (VOCs) and semi-volatile constituents (SVOCs) from wines. In this sense, and before they could be analysed by gas chromatography–quadrupole first stage masss spectrometry (GC–qMS), three different high-throughput miniaturized (ad)sorptive extraction techniques, based on solid phase extraction (SPE), microextraction by packed sorbents (MEPS) and solid phase microextraction (SPME), were studied for the first time together, for the extraction step. To achieve the most complete volatile and semi-volatile signature, distinct SPE (LiChrolut EN, Poropak Q, Styrene-Divinylbenzene and Amberlite XAD-2) and MEPS (C2, C8, C18, Silica and M1 (mixed C8-SCX)) sorbent materials, and different SPME fibre coatings (PA, PDMS, PEG, DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS), were tested and compared. All the extraction techniques were followed by GC–qMS analysis, which allowed the identification of up to 103 VOCs and SVOCs, distributed by distinct chemical families: higher alcohols, esters, fatty acids, carbonyl compounds and furan compounds. Mass spectra, standard compounds and retention index were used for identification purposes. SPE technique...