PMID- 33348272 OWN - NLM STAT- MEDLINE DCOM- 20210119 LR - 20210119 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1636 DP - 2021 Jan 11 TI - Organochlorine pesticide analysis in milk by gas-diffusion microextraction with gas chromatography-electron capture detection and confirmation by mass spectrometry. PG - 461797 LID - S0021-9673(20)31071-2 [pii] LID - 10.1016/j.chroma.2020.461797 [doi] AB - 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 microg 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. CI - Copyright (c) 2020. Published by Elsevier B.V. FAU - Lobato, Alnilan AU - Lobato A AD - Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo (USP), Sao Paulo - SP, Brazil. FAU - Fernandes, Virginia Cruz AU - Fernandes VC AD - REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto (ISEP), Instituto Politecnico do Porto, Porto, Portugal. Electronic address: virginiacruz@graq.isep.ipp.pt. FAU - Pacheco, Joao G AU - Pacheco JG AD - REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto (ISEP), Instituto Politecnico do Porto, Porto, Portugal. FAU - Delerue-Matos, Cristina AU - Delerue-Matos C AD - REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto (ISEP), Instituto Politecnico do Porto, Porto, Portugal. FAU - Goncalves, Luis Moreira AU - Goncalves LM AD - Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo (USP), Sao Paulo - SP, Brazil. Electronic address: lmgoncalves@iq.usp.br. LA - eng PT - Journal Article DEP - 20201210 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Hydrocarbons, Chlorinated) RN - 0 (Pesticide Residues) RN - 0 (Pesticides) SB - IM MH - Animals MH - Diffusion MH - *Electrons MH - Gas Chromatography-Mass Spectrometry/*methods MH - Hydrocarbons, Chlorinated/*analysis MH - Milk/*chemistry MH - Pesticide Residues/analysis MH - Pesticides/*analysis MH - Reproducibility of Results OTO - NOTNLM OT - Dairy products OT - Food quality OT - Microextraction OT - Persistent organic pollutants OT - Sample preparation OT - Separation COIS- Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. EDAT- 2020/12/22 06:00 MHDA- 2021/01/20 06:00 CRDT- 2020/12/21 20:16 PHST- 2020/09/23 00:00 [received] PHST- 2020/11/09 00:00 [revised] PHST- 2020/12/08 00:00 [accepted] PHST- 2020/12/22 06:00 [pubmed] PHST- 2021/01/20 06:00 [medline] PHST- 2020/12/21 20:16 [entrez] AID - S0021-9673(20)31071-2 [pii] AID - 10.1016/j.chroma.2020.461797 [doi] PST - ppublish SO - J Chromatogr A. 2021 Jan 11;1636:461797. doi: 10.1016/j.chroma.2020.461797. Epub 2020 Dec 10.