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Validação de um Método para a Análise de Resíduos de Pesticidas em Alimentos para Lactentes e Crianças Pequenas por GC-ECD
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Os alimentos para lactentes e crianças pequenas são produtos produzidos especialmente para este grupo de consumidores vulneráveis. Devem por isso cumprir exigências específicas da segurança ali-mentar, entre as quais os requisitos em matéria de controlo de resíduos de pesticidas.
Assim, a presente dissertação tem como objetivo validar o método analítico, por cromatografia gasosa com um detetor de captura de eletrões acoplado, para determinar a capacidade do mesmo quan-tificar seis pesticidas organoclorados (Aldrina, Dieldrina, Heptacloro, Heptacloro Epóxido (trans), He-xaclorobenzeno e Nitrofena) em três matrizes distintas: os baby food, os cereais e as fórmulas. De modo a extrair os resíduos destes pesticidas presentes nestas amostras é utilizado o método de extração QuE-ChERS.
A Direção Geral da Saúde e da Segurança dos Alimentos, como organismo de segurança alimen-tar da Comissão Europeia, estabelece um limite de resíduo de 0,003 mg pesticida/kg produto (3 ppb) para os pesticidas e matrizes em estudo, de acordo com o Regulamento 2016/127 da CE.
Ao longo da validação foram realizados ensaios de quantificação e de linearidade, em solvente, em que foi possível verificar que quase todos os resíduos (exceto o Heptacloro) apresentam uma resposta linear e que são quantificáveis na gama de trabalho escolhida, com limites de quantificação a variar entre 0,0005 mg/kg (0,5 ppb) para o Hexaclorobenzeno e 0,0105 mg/kg (10,5 ppb) para o Heptacloro. Ensaios de recuperação permitiram obter resultados sobre a precisão, exatidão e robustez através do desenho de experiências de Plackett-Burman. Verificou-se que a recuperação média dos resíduos foi de 80 %, que o método é robusto e que a estabilidade dos analitos, a 3 ºC e à temperatura ambiente, encontra-se entre 91-120 %. Por fim, na estimativa da incerteza foi possível verificar que a incerteza relativa expandida deste método é inferior a 50 % para todos os analitos em estudo.
Foods for infants and young children are products produced especially for this group of vulnerable con-sumers. They must therefore comply with specific food safety requirements, including requirements for the control of pesticide residues. Thus, the present dissertation aims to validate the analytical method, by gas chromatography with a coupled electron capture detector, to determine its ability to quantify six organochlorine pesticides (Al-drin, Dieldrin, Heptachlor, Heptachlor Epoxide (trans), Hexachlorobenzene and Nitrofen) in three dif-ferent matrices: baby food, cereals and formulas. In order to extract the residues of these pesticides present in the samples, the QuEChERS extraction method is used. The General Directorate of Health and Food Safety, as a food safety agency of the European Commis-sion, establishes a residue limit of 0.003 mg pesticide/kg product (3 ppb) for pesticides and matrices under study, in according to EC Regulation 2016/127. During the validation, quantification and linearity tests were carried out, in solvent, in which it was possible to verify that almost all residues (except for Heptachlor) had a linear response and that is pos-sible to quantify them in the chosen working range, with limits of quantification ranging from 0.0005 mg/kg (0.5 ppb) for Hexachlorobenzene to 0.0105 mg/kg (10.5 ppb) for Heptachlor. Recovery tests allowed obtaining results on precision, accuracy and robustness through the design of Plackett-Burman experiments. It was found that the average recovery of residues was 80 %, that the method is robust and that the stability of the analytes, at 3 ºC and at room temperature, is between 91-120 %. Finally, in the uncertainty estimation, it was possible to verify that the expanded relative uncertainty of this method is less than 50 % for all analytes under study.
Foods for infants and young children are products produced especially for this group of vulnerable con-sumers. They must therefore comply with specific food safety requirements, including requirements for the control of pesticide residues. Thus, the present dissertation aims to validate the analytical method, by gas chromatography with a coupled electron capture detector, to determine its ability to quantify six organochlorine pesticides (Al-drin, Dieldrin, Heptachlor, Heptachlor Epoxide (trans), Hexachlorobenzene and Nitrofen) in three dif-ferent matrices: baby food, cereals and formulas. In order to extract the residues of these pesticides present in the samples, the QuEChERS extraction method is used. The General Directorate of Health and Food Safety, as a food safety agency of the European Commis-sion, establishes a residue limit of 0.003 mg pesticide/kg product (3 ppb) for pesticides and matrices under study, in according to EC Regulation 2016/127. During the validation, quantification and linearity tests were carried out, in solvent, in which it was possible to verify that almost all residues (except for Heptachlor) had a linear response and that is pos-sible to quantify them in the chosen working range, with limits of quantification ranging from 0.0005 mg/kg (0.5 ppb) for Hexachlorobenzene to 0.0105 mg/kg (10.5 ppb) for Heptachlor. Recovery tests allowed obtaining results on precision, accuracy and robustness through the design of Plackett-Burman experiments. It was found that the average recovery of residues was 80 %, that the method is robust and that the stability of the analytes, at 3 ºC and at room temperature, is between 91-120 %. Finally, in the uncertainty estimation, it was possible to verify that the expanded relative uncertainty of this method is less than 50 % for all analytes under study.
Descrição
Palavras-chave
Validação de Métodos Pesticidas Cromatografia Gasosa Detetor de Captura de Eletrões Limite Máximo Resíduo QuEChERS