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Desenvolvimento de um Método Multiresíduo para a Análise de Pesticidas em Alimentos de Alto Teor em Gordura por GCMS/MS na SGS Portugal
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Os frutos secos são alimentos com elevado valor nutricional e importantes para uma alimentação
saudável, devido à presença de ácidos gordos e antioxidantes na sua composição. O crescimento do setor
agrícola e o aumento das exigências alimentares, têm levado a uma maior aplicação de pesticidas nas
produções agrícolas. Os resíduos de pesticidas presentes nos alimentos constituem uma ameaça para a
saúde pública, portanto, é importante desenvolver métodos de análise de resíduos de pesticidas em
produtos alimentares que garantam o cumprimento dos limites máximos de resíduos estipulados pela
União Europeia. Assim, foi desenvolvido e otimizado um método multiresíduo para a análise de
pesticidas em matrizes com elevado teor em gordura por cromatografia gasosa acoplada a um
espectrómetro de massa quadrupolo triplo (GC-MS/MS). A otimização do processo de extração do
método QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) permitiu ultrapassar os
problemas associados à complexidade das matrizes com elevado teor de gordura, através de uma etapa
de limpeza em fase sólida dispersiva (d-SPE). O método foi validado para os pesticidas clorfenvinfos e
malatião e para as matrizes amêndoa e amendoim, seguindo as diretrizes do guia SANTE/11312/2021.
O método apresenta uma boa linearidade (R2 > 0,995), dentro da gama de trabalho de 5 a 100 ppb, e
demonstra ser específico e seletivo na deteção do clorfenvinfos e do malatião para ambas as matrizes
em estudo. O limite de deteção (LD) do método é de 0,004 mg/kg e o limite de quantificação (LQ)
corresponde a 0,01 mg/kg. As matrizes avaliadas apresentam boas taxas de recuperação no intervalo de
70 a 120%. O coeficiente de variação (CV) varia entre 3,50% e 10,85% para a repetibilidade e entre
9,07% e 11,28% para a precisão intermédia. A incerteza do método é inferior a 50%. Os resultados da
validação encontram-se dentro dos critérios do SANTE/11312/2021 e o método pode ser aplicado a
análises de rotina, pois permite quantificar os pesticidas a valores inferiores ao LQ com boas taxas de
recuperação.
Dried fruits are foods with high nutritional value and are important for a healthy diet, due to the presence of fatty acids and antioxidants in their composition. The growth of the agricultural sector and the increase in food needs led to a greater application of pesticides in agricultural production. Pesticide residues present a threat to public health in specific foods, therefore, it is important to develop methods for analyzing pesticide residues in food products that guarantee compliance with the maximum residue limits stipulated by the European Union. Thus, a multiresidue method was developed and optimized for the analysis of pesticides in high oil matrices via gas chromatography coupled to a triple quadrupole mass spectrometer (GC-MS/MS). The optimization of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction method prevented possible problems associated with the complexity of high oil content matrices, through a dispersive solid-phase cleaning step (d-SPE). The method was validated for the pesticides chlorfenvinfos and malathion and for almond and peanut matrices, following the guidelines of the SANTE/11312/2021 guide. The method has good linearity (R2 > 0.995), within the working range of 5 to 100 ppb and has proven to be specific and selective in the detection of chlorfenvinphos and malathion for both matrices under study. The detection limit (LD) of the method is 0.004 mg/kg and the limit of quantification (LQ) corresponds to 0.01 mg/kg. The evaluated matrices present good recovery rates in the range of 70 to 120%. The coefficient of variation (CV) varies between 3.50% and 10.85% for repeatability and between 9.07% and 11.28% for intermediate precision. The uncertainty of the method is less than 50%. The validation results meet the SANTE/11312/2021 criteria and the method can be applied to routine analyses, as it allows pesticides to be quantified at values below the LQ with good recovery rates.
Dried fruits are foods with high nutritional value and are important for a healthy diet, due to the presence of fatty acids and antioxidants in their composition. The growth of the agricultural sector and the increase in food needs led to a greater application of pesticides in agricultural production. Pesticide residues present a threat to public health in specific foods, therefore, it is important to develop methods for analyzing pesticide residues in food products that guarantee compliance with the maximum residue limits stipulated by the European Union. Thus, a multiresidue method was developed and optimized for the analysis of pesticides in high oil matrices via gas chromatography coupled to a triple quadrupole mass spectrometer (GC-MS/MS). The optimization of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction method prevented possible problems associated with the complexity of high oil content matrices, through a dispersive solid-phase cleaning step (d-SPE). The method was validated for the pesticides chlorfenvinfos and malathion and for almond and peanut matrices, following the guidelines of the SANTE/11312/2021 guide. The method has good linearity (R2 > 0.995), within the working range of 5 to 100 ppb and has proven to be specific and selective in the detection of chlorfenvinphos and malathion for both matrices under study. The detection limit (LD) of the method is 0.004 mg/kg and the limit of quantification (LQ) corresponds to 0.01 mg/kg. The evaluated matrices present good recovery rates in the range of 70 to 120%. The coefficient of variation (CV) varies between 3.50% and 10.85% for repeatability and between 9.07% and 11.28% for intermediate precision. The uncertainty of the method is less than 50%. The validation results meet the SANTE/11312/2021 criteria and the method can be applied to routine analyses, as it allows pesticides to be quantified at values below the LQ with good recovery rates.
Descrição
Tese de Mestrado, Química Tecnológica, 2024, Universidade de Lisboa, Faculdade de Ciências
Palavras-chave
Clorfenvinfos Malatião GC-MS/MS Validação de Métodos QuEChERS Teses de mestrado - 2024