Organochlorine pesticide analysis in milk by gas-diffusion microextraction with gas chromatography-electron capture detection and confirmation by mass spectrometry

Autor(es)

Lobato, Alnilan ^[1] ; Fernandes, Virginia Cruz ^[2] ; Pacheco, Joao G. ^[2] ; Delerue-Matos, Cristina ^[2] ; Goncalves, Luis Moreira ^[1]

Afiliação do(s) autor(es)

^[1] Univ Sao Paulo, Dept Quim Fundamental, Inst Quim, Sao Paulo, SP - Brazil

^[2] Inst Politecn Porto, Inst Super Engn Porto ISEP, REQUIMTE LAQV, Porto - Portugal

• Tipo de documento: Artigo Científico
• Fonte: Journal of Chromatography A; v. 1636, JAN 11 2021.
• Citações Web of Science: 4

Resumo

Organochlorine pesticides (OCPs) are synthetic compounds less used nowadays due to their toxicity combined with slow degradation which leads to accumulation in the environment. Gas-diffusion microextraction (GDME) was employed prior to gas chromatography with electron capture detection (GC-ECD) and mass spectrometry (GC-MS). For the first time, the low-cost, eco-friendly GDME system was used to extract the OCPs directly from milk samples and associated with GC-ECD. Parameters that affect GDME's performance (extract volume, extraction time, and temperature) were optimized. The calibration curves of all OCPs (alpha- and beta-hexachlorocyclohexane, lindane, hexachlorobenzene, p,p'-DDE, aldrin, dieldrin, and alpha-endosulfan) had coefficients of determination (r(2)) ranging from 0.991 to 0.995, and limits of detection (LODs) values ranging from 3.7 to 4.8 mu g L-1. This method also provided satisfactory values for precision with relative standard deviations (RSDs) lower than 10% and recoveries above 90%. As a proof-of-concept, several commercial milk samples were analyzed, aldrin was found in one of them but below the maximum residue limits. (C) 2020 Elsevier B.V. All rights reserved. (AU)

• Processo FAPESP: 18/14425-7 - Um novo rumo sinérgico para a microextração por difusão gasosa (GDME) fazendo uso de polímeros com impressão molecular (MIPs)
• Beneficiário: Luís Francisco Moreira Gonçalves
• Modalidade de apoio: Auxílio à Pesquisa - Jovens Pesquisadores
• Processo FAPESP: 19/11214-8 - Recurso à eletroforese capilar após extração por GDME-MIPs para a determinação de aldeídos
• Beneficiário: Alnilan Cristina Barros Lobato
• Modalidade de apoio: Bolsas no Brasil - Mestrado