Dynamic Microwave-assisted Extraction Online Coupled with QuEChERS for the Determination of Organophosphorus Pesticides
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doi: 10.1007/s40242-020-9083-8
Dynamic Microwave-assisted Extraction Online Coupled with QuEChERS for the Determination of Organophosphorus Pesticides in Cereals by Gas Chromatography LI Guijie1, LIU Chang3, LIU Hongcheng1, WANG Dawei1* and DING Lan2* 1. College of Food Science, Jilin Agricultural University, Changchun 130118, P. R. China; 2. College of Chemistry, Jilin University, Changchun 130012, P. R. China; 3. Jilin Province Product Quality Supervision and Inspection Institute, Changchun 130103, P. R. China 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, C 18 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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Introduction
Organophosphorus pesticides(OPPs) are usually applied to effectively control pests in agriculture. As a result, there are increasing health and security concerns all over the world[1,2]. The European Commission has set clear maximum residue limits for most OPPs in cereals, usually no more than 0.01 mg/kg[Regulation(EC) No.396/2005]. China’s National Standard GB 2763-2016 stipulates that the maximum residues of OPPs in cereals should be within the range of 0.02―8 mg/kg. Taking the above reasons into account, a simple, fast and reliable method for OPPs in cereals is indispensable to be established. Detection methods of OPPs mainly include gas chromatography(GC)[3―6], gas chromatography-mass spectrometry (GC-MS)[7,8], liquid chromatography(LC)[9] and liquid chromatography-tandem mass spectrometry(LC-MS)[10]. Among the methods, GC has the advantages of simple operation, low cost, rapid analysis and high sensitivity with flame photometric detector(FPD) for the detection of OPPs. Common extraction methods o
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