http://dx.doi.org/10.5935/sc.2018.001
Multiresidue determination of pesticides in sweet peppers by LC-MS/MS using Si-Al(PMTDS) as a sorbent for extraction by MSPD
Morais EHC et al.
Palavras-chave: cromatografia líquida acoplada à espectrometria de massas sequencial; dispersão da matriz em fase sólida; pimentões; agrotóxicos; validação.
Resumo: Um método rápido, eficaz e ambientalmente seguro para determinação multirresíduo de agrotóxicos em amostras de pimentões verdes usando dispersão da matriz em fase sólida com um novo dispersante, poli(metiltetradecilsiloxano), imobilizado termicamente em sílica recoberta com alumina, Si-Al(PMTDS), e determinação por cromatografia líquida acoplada à espectrometria de massas sequencial foi desenvolvido e validado. O desempenho do novo dispersante foi comparado com outros como C18 e SiO2. Também foram avaliadas acetonitrila e acetato de etila como solventes de extração. O sorvente à base de Si-Al(PMTDS) forneceu resultados semelhantes aos sorventes comerciais testados em termos de recuperação. No entanto, apenas o sorvente polimérico preparado no laboratório garantiu a seletividade da separação. Usando Si-Al(PMTDS) como dispersante na extração, as recuperações para quase todos os analitos ficaram na faixa de 70-120%, com coeficientes de variação inferiores a 20%, valores recomendáveis para a análise de resíduos de agrotóxicos em amostras complexas, demonstrando exatidão e precisão dos resultados para todos os analitos. Todos os limites de quantificação foram inferiores aos limites máximos de resíduos para os agrotóxicos analisados. O método desenvolvido foi aplicado em análises de pimentões verdes adquiridos no comércio. Alguns agrotóxicos autorizados foram encontrados, mas todos em níveis de concentração inferiores aos limites máximos de resíduos. No entanto, vários agrotóxicos não autorizados também foram encontrados. A preparação do sorvente Si-Al(PMTDS) é simples, reprodutível e o custo é compatível com sorventes comercialmente disponíveis utilizados na dispersão de matriz em fase sólida.
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