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Master's Dissertation
DOI
https://doi.org/10.11606/D.75.2022.tde-11112022-175627
Document
Author
Full name
Mariá Del Bianco Luppi
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Carlos, 2022
Supervisor
Committee
Santos Neto, Álvaro José dos (President)
Nassur, Maria Eugenia Queiroz
Nazário, Carlos Eduardo Domingues
Title in Portuguese
Estudos de derivatização direta de anfetaminas no injetor em GC-MS
Keywords in Portuguese
anfetaminas
cromatografia gasosa
derivatização
injection port derivatization
Abstract in Portuguese
A cromatografia gasosa acoplada à espectrometria de massas apresenta-se como ferramenta com aplicação em diversos segmentos: farmacêutico, cosmético, forense e petroquímico, possibilitando a separação e identificação de moléculas de interesse. A crescente necessidade de monitoramento e identificação de substâncias psicoativas pode ser percebida pela implementação da portaria do Ministério do Trabalho e Previdência Social MTPS No 116 de 13/11/2015 que regulamenta a realização de exames toxicológicos em motoristas profissionais do transporte rodoviário coletivo de passageiros e do transporte rodoviário de cargas, que traz a demanda por métodos analíticos capazes de auxiliar na identificação e quantificação dessas substâncias. Dentre as substâncias psicoativas contempladas pelo exame toxicológico exigido pelo do Ministério do Trabalho e Previdência Social MTPS No 116 de 13/11/2015, foram selecionadas: anfetamina, metanfetamina, 3,4- metilenodioximetanfetamina (MDMA) e 3,4-metilenodioxianfetamina (MDA) para o presente trabalho de estudos de derivatização direta de anfetaminas no injetor. Foi avaliada a aplicação da derivatização on-line (injection port derivatization) para determinação de anfetaminas em amostras de cabelo. Os derivatizantes anidridro acético (AA), N-metil-bis-trifluoroacetamida (MBTFA) e anidrido heptafluorobutírico (HFBA) foram avaliados para aplicação da derivatização on-line. As análises foram feitas pela técnica de cromatografia gasosa acoplada a espectrometria de massas (GC-MS) e foram avaliados os parâmetros de fluxo de purga, temperatura do injetor e volume de derivatizante utilizados. Dois protocolos de extração diferentes foram testados, e o protocolo com melhor recuperação foi aplicado a uma amostra real de cabelo. Os resultados foram satisfatórios e mostraram o potencial de utilização do N-metil-bis-trifluoroacetamida (MBTFA) como derivatizante em preparos com derivatização direta no injetor para determinação de anfetaminas em cabelo, com possibilidade futura de validação de método para aplicação em rotina de laboratório.
Title in English
Study of direct derivatization of amphetamines in GC-MS injector
Keywords in English
amphetamines
derivatization
gas chromatography
injection port derivatization
Abstract in English
Gas chromatography coupled to mass spectrometry is presented as a tool with potential applications in various segments: pharmaceutical, cosmetic, forensics, and petrochemical, allowing the separation and identification of molecules of interest. The growing need of monitoring and identification of psychoactive substances can be noted by the implementation of the ordinance no. 166 from Ministério do Trabalho e Previdência Social MTPS (Ministry of Labor and Social Security) from 11/13/2015, that regulates the execution of toxicological exams on professional drivers of collective passenger transport and road freight transport, that creates the demand for analytical methods that are able to help the identification and quantification of those substances. Among the psychoactive substances included in the toxicological exam demanded by ordinance no. 166 from Ministério do Trabalho e Previdência Social MTPS (Ministry of Labor and Social Security) from 11/13/2015, were selected: amphetamine, methamphetamine, 3,4- methylenedioxymethamphetamine (MDMA) and 3,4-methylenedioxyamphetamine (MDA) for the present work of direct derivation studies of amphetamines in the injector. The application of the online derivation was assessed (injection port derivatization) to determine amphetamines in hair samples. The derivativesacetic anhydride (AA), N-methyl-bis-trifluoroacetamide (MBTFA) and heptafluorobutyric anhydride were assessed for the application of the online derivatization. The analyses were made by gas chromatography coupled to mass spectrometry (GC- MS), and the parameters analyzed were: purge flow, injector temperature, and volume of derivative used. Two different protocols of injection were assessed, and the protocol with the best recovery was applied to a real hair sample. The results were good and showed the potential of the use of N-methyl-bis-trifluoroacetamide (MBTFA) as derivative in preparations of direct derivatization in the injector to determine amphetamines in hair, with the possibility of a future method validation for the application in a laboratory routine.
 
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Publishing Date
2022-11-17
 
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