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Abstract(s)
A presente dissertação de mestrado encontra-se dividida em três capítulos. No primeiro e
segundo capítulo encontram-se descritos os estágios realizados, respetivamente, em farmácia
comunitária e farmácia hospitalar. São referidas as principais atividades desenvolvidas e
funções assumidas no Hospital Sousa Martins e na Farmácia Tavares, com destaque para a
importância crescente do farmacêutico em equipas multidisciplinares de saúde e como agente
de promoção de saúde pública.
No terceiro capítulo encontra-se descrito o trabalho de investigação desenvolvido no Centro
de Investigação em Ciências da Saúde da Universidade da Beira Interior.
A cannabis é a droga ilícita mais disponível e mais consumida a nível mundial, como tal tornase
necessário dotar os laboratórios de metodologias mais céleres e eficazes de forma a
identificar e quantificar estas substâncias psicoativas. O objetivo do trabalho de investigação
foi o desenvolvimento e validação de um método analítico usando microextração em seringa
empacotada e cromatografia gasosa acoplada à espetrometria de massa em tandem, para a
determinação e quantificação do delta-9-tetrahidrocanabinol, 11-hidroxi- delta-9-
tetrahidrocanabinol e 11-nor-9-carboxi-delta-9-tetrahidrocanabinol em amostras de plasma
humano. É de salientar que esta é a primeira vez que estes compostos são determinados em
amostras de plasma com recurso à microextração em seringa empacotada.
A elevada quantidade de interferentes biológicos existentes na matriz torna a preparação das
amostras um passo fundamental no processo analítico. Desta forma procedeu-se à otimização
da técnica extrativa usando o planeamento fatorial, uma ferramenta estatística aplicada ao
processo de decisão e que avalia de forma multivariada os fatores intervenientes na extração.
As condições finais otimizadas foram: diluição da amostra (1:20), número de aspirações pelo
dispositivo (26), quantidade de ácido acético numa solução de lavagem (3%), quantidade de
metanol noutra solução de lavagem (5%) e quantidade de hidróxido de amónio na solução de
eluição (10%).
O método foi validado seguindo critérios internacionais e os parâmetros estudados incluíram
linearidade, seletividade, limites de deteção (LOD) e quantificação (LLOQ), precisão e
exatidão. O procedimento foi linear para o intervalo de concentrações de 0,1 (limite inferior
de quantificação - LLOQ) até 30 ng/mL, com coeficientes de determinação (R2) superiores a
0,99 para todos os analitos. Precisões intra- e inter-dia foram tipicamente inferiores a 15%
para todos os analitos a todas as concentrações estudadas, enquanto a exatidão se situou
dentro do intervalo de ±15%. As recuperações variaram entre 53% e 78%. O método validado mostrou ser aplicável à análise de amostras reais, sendo então uma
ferramenta vantajosa não só no âmbito de análises de toxicologia clínica e forense, mas
também em análises de despiste de consumo de cannabis e derivados.
This Master thesis is divided into three chapters. In the first and second chapters the conducted internships are described, respectively, in community pharmacy and hospital pharmacy. Here the main activities developed and duties undertaken at Hospital Sousa Martins and at Farmácia Tavares are referred, with emphasis to the growing importance of the pharmacist in multidisciplinary health care teams and as a promoting agent of public health. The third chapter describes the investigation work developed at Centro de Investigação em Ciências da Saúde da Universidade da Beira Interior. Cannabis is the most available and consumed illegal drug worldwide, accordingly it becomes necessary to provide laboratories with more prompt and effective methodologies to identify and quantify these psychoactive substances. The goal of this research work was the development and validation of an analytic method using microextraction by packed sorbent and gas chromatography coupled to tandem mass spectrometry, for determination and quantification of delta-9-tetrahydrocannabinol, 11-hydroxi-delta-9-tetrahydrocannabinol and 11-nor-9-carboxi-delta-9-tetrahydrocannabinol in human plasma samples. It should be noted that this is the first time that these compounds are determined in plasma samples through microextraction by packed sorbent. The high quantity of existing interfering compounds in biological matrices makes sample preparation the fundamental step in the analytic process. Thus the optimization of the extractive technique using factorial design, a statistic tool applied to the decision process and which evaluates the extraction factors in a multivaried way. The final optimized conditions were: dilution of the sample (1:20), number of strokes (26), amount of acetic acid in a washing solution (3%), amount of methanol in another washing solution (5%) and amount of ammonium hydroxide in the elution solution (10%). The method was validated following international criteria and the studied parameters included linearity, selectivity, limits of detection (LOD) and quantification (LLOQ), precision and accuracy. The procedure was linear for concentrations ranging from 0.1 (lower limit of quantification – LLOQ) to 30 ng/mL, with determination coefficients (R2 ) higher than 0.99 for all analytes. Intra- and inter-day precisions were typically lower than 15% for all analytes at all studied concentrations, while the accuracy remained between a ±15% interval. Recoveries ranged from 53% to 78%. The method was shown to be applicable to real samples, therefore being a powerful tool not only within clinical and forensic toxicology, but also assessing cannabis and derived products consumption.
This Master thesis is divided into three chapters. In the first and second chapters the conducted internships are described, respectively, in community pharmacy and hospital pharmacy. Here the main activities developed and duties undertaken at Hospital Sousa Martins and at Farmácia Tavares are referred, with emphasis to the growing importance of the pharmacist in multidisciplinary health care teams and as a promoting agent of public health. The third chapter describes the investigation work developed at Centro de Investigação em Ciências da Saúde da Universidade da Beira Interior. Cannabis is the most available and consumed illegal drug worldwide, accordingly it becomes necessary to provide laboratories with more prompt and effective methodologies to identify and quantify these psychoactive substances. The goal of this research work was the development and validation of an analytic method using microextraction by packed sorbent and gas chromatography coupled to tandem mass spectrometry, for determination and quantification of delta-9-tetrahydrocannabinol, 11-hydroxi-delta-9-tetrahydrocannabinol and 11-nor-9-carboxi-delta-9-tetrahydrocannabinol in human plasma samples. It should be noted that this is the first time that these compounds are determined in plasma samples through microextraction by packed sorbent. The high quantity of existing interfering compounds in biological matrices makes sample preparation the fundamental step in the analytic process. Thus the optimization of the extractive technique using factorial design, a statistic tool applied to the decision process and which evaluates the extraction factors in a multivaried way. The final optimized conditions were: dilution of the sample (1:20), number of strokes (26), amount of acetic acid in a washing solution (3%), amount of methanol in another washing solution (5%) and amount of ammonium hydroxide in the elution solution (10%). The method was validated following international criteria and the studied parameters included linearity, selectivity, limits of detection (LOD) and quantification (LLOQ), precision and accuracy. The procedure was linear for concentrations ranging from 0.1 (lower limit of quantification – LLOQ) to 30 ng/mL, with determination coefficients (R2 ) higher than 0.99 for all analytes. Intra- and inter-day precisions were typically lower than 15% for all analytes at all studied concentrations, while the accuracy remained between a ±15% interval. Recoveries ranged from 53% to 78%. The method was shown to be applicable to real samples, therefore being a powerful tool not only within clinical and forensic toxicology, but also assessing cannabis and derived products consumption.
Description
Keywords
Farmácia comunitária - Gestão - Estágio pedagógico Farmácia hospitalar - Gestão - Estágio pedagógico Microextração em seringa empacotada Plasma Canabinóides Cromatografia gasosa Espectrometria de massa
Citation
Publisher
Universidade da Beira Interior