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Análise de substâncias de abuso utilizando novas configurações de microextração em fase sólida e cromatografia gasosa-espetrometria de massa : estudo de prova de conceito
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Authors
Abstract(s)
O consumo de substâncias de abuso é considerado um problema de saúde pública de grande importância, uma vez que limita a vida dos seus consumidores e desvia recursos de várias áreas da sociedade.
Tendo em conta os problemas relacionados com o consumo das substâncias de abuso e os seus efeitos negativos consequentes, justifica-se cada vez mais o seu estudo, bem como o desenvolvimento de novos métodos analíticos, que permitam uma melhor monitorização das mesmas em contexto clínico, legal ou epidemiológico.
Neste sentido, na presente dissertação realizaram-se diversos ensaios experimentais com o objetivo de avaliar a adequabilidade de novos métodos de preparação de amostras, baseadas em microextração em fase sólida (SPME), para a deteção de substâncias de abuso em matrizes biológicas, visando a sua potencial introdução como metodologias alternativas verdes.
A análise quantitativa e qualitativa foi realizada por duas técnicas cromatográficas utilizando analisadores de massa diferentes: cromatografia gasosa hifenada à espetrometria de massa utilizando um analisador de tempo de voo (GC-TOF/MS) e cromatografia gasosa acoplada à espetrometria de massa em tandem (GC-TQ/MS), utilizando um triplo quadrupolo.
Os dados obtidos indicam que a técnica de SPME com fibras de configuração clássicas e configuração tips é um método seletivo para a determinação dos compostos cocaína, cocaetileno, fentanilo e norfentanilo. Os resultados experimentais indicam igualmente que esta técnica de preparação de amostra é promissora para estas substâncias de abuso, sendo necessários estudos adicionais de otimização do método. Globalmente, os resultados demonstraram que as metodologias propostas são operacionalmente simples, amigas do ambiente e com um custo-benefício vantajoso.
O investimento inicial na aquisição dos dispositivos baseados em SPME é rapidamente compensado pela sua capacidade de reutilização e baixo consumo de amostra e solventes orgânicos durante o ciclo analítico. Por outro lado, os métodos de preparação de amostra desenvolvidas ao longo do projeto de investigação, demonstram ser eficazes para o enriquecimento dos analitos alvo em matrizes biológicas, ao mesmo tempo que não descuram os princípios da química analítica verde e performance analítica.
Substance abuse is considered a public health problem of great importance, since it limits the lives of its users and diverts resources from various areas of society. Considering the problems related to substance abuse and its consequent negative effects, there is a growing need to study it and to develop new analytical methods that allow a better monitoring of these substances in clinical, legal or epidemiological context. In this sense, in the present dissertation several experimental tests were carried out to evaluate the suitability of new sample preparation methods, based on solid phase microextraction (SPME), for the detection of substances of abuse in biological matrices, aiming at their potential introduction as alternative green methodologies. Quantitative and qualitative analysis was performed by two chromatographic techniques using different mass analyzers: gas chromatography hyphenated to mass spectrometry using a time-of-flight analyzer (GC-TOF/MS) and gas chromatography coupled to tandem mass spectrometry (GC-TQ/MS) using a triple quadrupole. The data obtained indicate that the SPME technique with classic configuration fibers and tips configuration is a selective method for the determination of the compounds cocaine, cocaethylene, fentanyl and norfentanyl. The experimental results also indicate that this sample preparation technique is promising for these substances of abuse, but further method optimization studies are required. Overall, the results demonstrated that the proposed methodologies are operationally simple, environmentally friendly and cost-effective. The initial investment in purchasing the SPME-based devices is quickly offset by their reusability and low consumption of sample and organic solvents during the analytical cycle. On the other hand, the sample preparation methods developed throughout the research project, prove to be effective for the enrichment of target analytes in biological matrices, while not neglecting the principles of green analytical chemistry and analytical performance.
Substance abuse is considered a public health problem of great importance, since it limits the lives of its users and diverts resources from various areas of society. Considering the problems related to substance abuse and its consequent negative effects, there is a growing need to study it and to develop new analytical methods that allow a better monitoring of these substances in clinical, legal or epidemiological context. In this sense, in the present dissertation several experimental tests were carried out to evaluate the suitability of new sample preparation methods, based on solid phase microextraction (SPME), for the detection of substances of abuse in biological matrices, aiming at their potential introduction as alternative green methodologies. Quantitative and qualitative analysis was performed by two chromatographic techniques using different mass analyzers: gas chromatography hyphenated to mass spectrometry using a time-of-flight analyzer (GC-TOF/MS) and gas chromatography coupled to tandem mass spectrometry (GC-TQ/MS) using a triple quadrupole. The data obtained indicate that the SPME technique with classic configuration fibers and tips configuration is a selective method for the determination of the compounds cocaine, cocaethylene, fentanyl and norfentanyl. The experimental results also indicate that this sample preparation technique is promising for these substances of abuse, but further method optimization studies are required. Overall, the results demonstrated that the proposed methodologies are operationally simple, environmentally friendly and cost-effective. The initial investment in purchasing the SPME-based devices is quickly offset by their reusability and low consumption of sample and organic solvents during the analytical cycle. On the other hand, the sample preparation methods developed throughout the research project, prove to be effective for the enrichment of target analytes in biological matrices, while not neglecting the principles of green analytical chemistry and analytical performance.
Description
Dissertação para obtenção do grau de Mestre no Instituto Universitário Egas Moniz
Keywords
Substâncias de abuso Preparação de amostras SPME com fibras clássicas e tips Matrizes biológicas