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

•Organochlorine pesticides (OCPs) were extracted and analyzed without derivatization.•Extraction was performed by gas-diffusion microextraction (GDME).•GDME-GC-ECD and GDME-GC-MS was applied in the analysis of OCPs in milk.•An alternative low-cost sample preparation system was successfully applied.•...

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Bibliographic Details
Published in:Journal of Chromatography A 2021-01, Vol.1636, p.461797, Article 461797
Main Authors: Lobato, Alnilan, Fernandes, Virgínia Cruz, Pacheco, João G., Delerue-Matos, Cristina, Gonçalves, Luís Moreira
Format: Article
Language:English
Subjects:
Dairy products
Food quality
Microextraction
Persistent organic pollutants
Sample preparation
Separation
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Summary:•Organochlorine pesticides (OCPs) were extracted and analyzed without derivatization.•Extraction was performed by gas-diffusion microextraction (GDME).•GDME-GC-ECD and GDME-GC-MS was applied in the analysis of OCPs in milk.•An alternative low-cost sample preparation system was successfully applied.•The obtained limits of detection were below the legal maximum residue limits. 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 (α- and β-hexachlorocyclohexane, lindane, hexachlorobenzene, p,p′-DDE, aldrin, dieldrin, and α-endosulfan) had coefficients of determination (r2) ranging from 0.991 to 0.995, and limits of detection (LODs) values ranging from 3.7 to 4.8 µg 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.
ISSN:0021-9673
DOI:10.1016/j.chroma.2020.461797