Dynamic Microwave-assisted Extraction Online Coupled with QuEChERS for the Determination of Organophosphorus Pesticides in Cereals by Gas Chromatography

Abstract

A rapid analytical method was first developed to detect organophosphorus pesticides(OPPs) in cereals, which used dynamic microwave assisted extraction(DMAE) coupled online with a modified quick, easy, cheap, effective, rugged, and safe(QuEChERS) method. Cereals samples were mixed with a certain amount of quartz, C18 and primary second amine(PSA), and extracted successively with the acetonitrile-water solution(80%, V/V) under microwave irradiation. The obtained eluate was directly introduced into a collection tube containing NaCl and MgSO₄. Finally, the supernate was evaporated and reconstructed, and determined by gas chromatographic spectrometry. Some factors affecting the experimental results were studied and optimized. The extraction and purification processes were carried out coinstantaneously and 12 samples could be treated in one step in 4 min. Low limits of detection(0.43–1.31 µg/kg) for OPPs were obtained in cereals. The relative standard deviations(RSDs) were 2.1%–9.3%. The recoveries of OPPs ranged from 76.1% to 100.2%. By combining the advantages of DMAE with QuEChERS, the sample pretreatment process was simple to operate, with little amount of organic solvent. The whole extraction process was completed in a closed environment, therefore it was very appropriate for daily analysis of OPPs in cereals.

Keywords

Dynamic microwave-assisted extraction / Quick, easy, cheap, effective, rugged, and safe(QuEChERS) / Gas chromatographic spectrometry / Organophosphorus pesticide / Cereal

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