Development and validation of a modified QuEChERS method based on magnetic zirconium dioxide microspheres for the determination of 52 pesticides in oil crops by gas chromatography tandem mass spectrometry

作者：Lu, Wei; Peng, Xitian^*; Shen, Jing; Hu, Xizhou; Peng, Lijun; Feng, Yuqi

来源：Analytical Methods, 2015, 7(20): 8663-8672.

DOI：10.1039/c5ay01293g

• SOLID-PHASE EXTRACTION
• MULTI-RESIDUE ANALYSIS
• LIQUID-CHROMATOGRAPHY
• VEGETABLE MATRICES
• GC-MS/MS
• CLEANUP
• AVOCADO
• HERBICIDES
• FRUITS
• AMINE

The residue analysis of pesticides in high-fat oil crops is a chaenging task because of the high amount of lipid co-extracts, which could seriously affect the extraction efficiency and the performance of instruments. In this study, a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method based on magnetic mesoporous ZrO2 microspheres (m-ZrO2@Fe3O4) and n-octadecylphosphonic acid modified magnetic microspheres (Fe3O4-OPA) was established for the determination of 52 pesticides in oil crops by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). The ability of m-ZrO2@Fe3O4 to remove fatty acids from acetonitrile extracts of oil crops has been evaluated. The results indicated that m-ZrO2@Fe3O4 showed better performance in the removal of fatty acids than that of PSA, a commonly used sorbent to remove acidic co-extracts in the QuEChERS method. The parameters affecting the cleanup performance including the amounts of m-ZrO2@Fe3O4 and Fe3O4-OPA were aka investigated. Under optimal conditions, the method was validated in four kinds of oil crops (peanuts, rapeseed, soybean and sesame) by GC-MS/MS. The linear correlation coefficients (R-2) of all four oil crops were higher than 0.9904. The limits of detection (LODs) were found to be in the range of 0.1-4.1 mu g kg(-1). The average recoveries of all analytes ranged from 69.1% to 120.0% (except p,p'-DDE, p,p'-DDD, o,p'-DDT and p,p'-DDT) with the intra-day and inter-day relative standard deviations (RSDs) less than 14.7% and 14.9%, respectively.

• 出版日期2015
• 单位武汉大学; 湖北省农业科学院