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Validação de um método em cromatografia líquida e gasosa acoplada a espetrometria de massa em Tandem (LC-MS/MS e GC- MS/MS) para deteção de pesticidas em ma- trizes complexas
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Resumo(s)
O chá verde, matriz complexa com benefícios para a saúde, amplamente consumido, é
sujeito à aplicação de pesticidas, exigindo métodos analíticos rigorosos para assegurar a sua
segurança alimentar. Devido ao risco que estes contaminantes representam para a saúde, de-
senvolveu-se um método analítico, num laboratório certificado, para a deteção de resíduos de
pesticidas.
A validação de um método requer primeiramente a preparação e extração das amostras,
com solventes adequados à polaridade, solubilidade e estabilidade da matriz, compatibilidade
com os equipamentos e eficiência na extração do analito. O processo de extração foi realizado
com o método QuEChERS,
quick, easy, cheap, effective, rugged, and safe, caracterizada como
a técnica de extração de amostras multiresiduos de pesticidas mais utilizada na indústria ali-
mentar. A respetiva análise decorreu em dois equipamentos distintos: cromatografia líquida
acoplada a um espetrómetro de massa triplo quadrupolo (LC-MS/MS) e cromatografia gasosa
acoplada a um espetrómetro de massa triplo quadrupolo (GC-MS/MS), onde se escolheram
um pesticida por equipamento, Azoxistrobina e Trifluralina, respetivamente.
Determinaram-se parâmetros de validação de modo a comprovar a capacidade do mé-
todo analítico para fornecer dados consistentes, confiáveis e precisos, a avaliação teve por base
os critérios de validação presentes no guia SANTE/11312/2021. Conclui-se que o método apre-
senta uma boa linearidade (R2 > 0,995), dentro da gama de trabalho de 2 a 100 ppb, e verifica-
se a especificidade e seletividade na deteção de ambos os pesticidas. Verificou-se que a matriz
em análise apresenta taxas de recuperação no intervalo de 70 a 120%. Um coeficiente de vari-
ação (CV) de 4,85% (Trifluralina) e 8,65% (Azoxistrobina) para a repetibilidade e 5,79% (Triflura-
lina) e 5,84% (Azoxistrobina) para a precisão intermédia. A incerteza do método apresenta
valores entre 12,10% e 12,56%. Conclui-se que os resultados da validação encontram-se dentro
dos critérios de aceitação do SANTE/11312/2021 e o método pode ser aplicado a análises de
rotina.
Green tea, a complex matrix with health benefits, widely consumed, is subject to pesticide application, requiring rigorous analytical methods to ensure its food safety. Due to the risk these contaminants pose to health, an analytical method has been developed in a certified laboratory for the detection of pesticide residues. The validation of a method first requires the preparation and extraction of samples, using solvents appropriate to the polarity, solubility, and stability of the matrix, compatibility with the equipment, and efficiency in the extraction of the analyte. The extraction process was per- formed using the QuEChERS method, which is quick, easy, cheap, effective, rugged, and safe, and is characterized as the most widely used technique for extracting multi-residue pesticide samples in the food industry. The respective analysis was performed on two different pieces of equipment: liquid chromatography coupled with a triple quadrupole mass spectrometer (LC- MS/MS) and gas chromatography coupled with a triple quadrupole mass spectrometer (GC- MS/MS), where one pesticide was chosen per equipment, Azoxystrobin and Trifluralin, respec- tively. Validation parameters were determined to verify the analytical method's ability to pro- vide consistent, reliable, and accurate data. The evaluation was based on the validation criteria presented in guide SANTE/11312/2021. It was concluded that the method has good linearity (R2 > 0.995) within the working range of 2 to 100 ppb, and specificity and selectivity in the detection of both pesticides were verified. It was found that the matrix under analysis has re- covery rates in the range of 70 to 120%. A coefficient variation (CV) of 4.85% (Trifluralin) and 8.65% (Azoxystrobin) for repeatability and 5.79% (Trifluralin) and 5.84% (Azoxystrobin) for in- termediate precision. The uncertainty of the method ranges from 12.10% to 12.56%. It is con- cluded that the validation results are within the acceptance criteria of SANTE/11312/2021 and the method can be applied to routine analyses.
Green tea, a complex matrix with health benefits, widely consumed, is subject to pesticide application, requiring rigorous analytical methods to ensure its food safety. Due to the risk these contaminants pose to health, an analytical method has been developed in a certified laboratory for the detection of pesticide residues. The validation of a method first requires the preparation and extraction of samples, using solvents appropriate to the polarity, solubility, and stability of the matrix, compatibility with the equipment, and efficiency in the extraction of the analyte. The extraction process was per- formed using the QuEChERS method, which is quick, easy, cheap, effective, rugged, and safe, and is characterized as the most widely used technique for extracting multi-residue pesticide samples in the food industry. The respective analysis was performed on two different pieces of equipment: liquid chromatography coupled with a triple quadrupole mass spectrometer (LC- MS/MS) and gas chromatography coupled with a triple quadrupole mass spectrometer (GC- MS/MS), where one pesticide was chosen per equipment, Azoxystrobin and Trifluralin, respec- tively. Validation parameters were determined to verify the analytical method's ability to pro- vide consistent, reliable, and accurate data. The evaluation was based on the validation criteria presented in guide SANTE/11312/2021. It was concluded that the method has good linearity (R2 > 0.995) within the working range of 2 to 100 ppb, and specificity and selectivity in the detection of both pesticides were verified. It was found that the matrix under analysis has re- covery rates in the range of 70 to 120%. A coefficient variation (CV) of 4.85% (Trifluralin) and 8.65% (Azoxystrobin) for repeatability and 5.79% (Trifluralin) and 5.84% (Azoxystrobin) for in- termediate precision. The uncertainty of the method ranges from 12.10% to 12.56%. It is con- cluded that the validation results are within the acceptance criteria of SANTE/11312/2021 and the method can be applied to routine analyses.
Descrição
Palavras-chave
Chá verde GC-MS/MS LC-MS/MS Pesticidas Validação