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Authors
Advisor(s)
Abstract(s)
Nos últimos dez anos o consumo de novas substâncias psicoativas (NSP) tem vindo a
aumentar sendo que têm sido introduzidas novas substâncias cada semana. O seu
consumo constitui um problema social e de saúde pública pelo que a análise toxicológica
se torna da maior importância. Neste documento descreve-se o desenvolvimento e
otimização de um método simples, rápido, sensível e com baixo consumo de solventes
orgânicos para a determinação da ketamina e do seu principal metabolito norketamina em
amostras de cabelo. O procedimento descrito incluiu a utilização de uma técnica
miniaturizada, a microextração em seringa empacotada (MEPS) bem como a
cromatografia de gases acoplada à espetrometria de massa em tandem (GC-MS/MS).
Prévio ao processo de clean-up, foi otimizado o processo de hidrólise. Foram também
otimizados os parâmetros que influenciam o processo de extração com recurso à
ferramenta estatística de desenho experimental (DOE). Os limites de deteção obtidos
foram de 0,01 e 0,05 ng/mg para a ketamina e norketamina, respetivamente. Quanto à
eficiência de extração, este parâmetro variou entre 32 e 60%. É importante salientar que
este é o primeiro método descrito que permite a determinação de ketamina e metabolito
com recurso à MEPS e GC-MS/MS em amostras de cabelo.
In the last ten years, the consumption of new psychoactive substances (NPS) has increased rapidly, with new substances being introduced every week. The consumption of these substances is considered a social and public health problem, so toxicological analysis plays a role of utmost importance. This thesis describes the development and optimization of a simple, rapid, sensitive, and low organic solvent consumption method for the determination of ketamine and its main metabolite, norketamine, in hair samples. The described procedure included a miniaturized technique, microextraction by packed sorbent (MEPS), as well as gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Before the clean-up process, the hydrolysis was optimized. The parameters influencing the extraction were also optimized using the statistical tool Design of Experiments (DOE). The detection limits obtained were 0.01 and 0.05 ng/mg for ketamine and norketamine, respectively. As for extraction efficiency, values between 32 and 60% were obtained. It is crucial to point out that this is the first described method that allows the determination of ketamine and metabolite using MEPS and GC-MS/MS in hair samples.
In the last ten years, the consumption of new psychoactive substances (NPS) has increased rapidly, with new substances being introduced every week. The consumption of these substances is considered a social and public health problem, so toxicological analysis plays a role of utmost importance. This thesis describes the development and optimization of a simple, rapid, sensitive, and low organic solvent consumption method for the determination of ketamine and its main metabolite, norketamine, in hair samples. The described procedure included a miniaturized technique, microextraction by packed sorbent (MEPS), as well as gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Before the clean-up process, the hydrolysis was optimized. The parameters influencing the extraction were also optimized using the statistical tool Design of Experiments (DOE). The detection limits obtained were 0.01 and 0.05 ng/mg for ketamine and norketamine, respectively. As for extraction efficiency, values between 32 and 60% were obtained. It is crucial to point out that this is the first described method that allows the determination of ketamine and metabolite using MEPS and GC-MS/MS in hair samples.
Description
Keywords
Cabelo Gc-Ms/Ms Ketamina Microextração em Seringa Empacotada Novas Substâncias Psicoativas