快速溶剂萃取在线凝胶渗透色谱-串联气质联 用法测定大豆中53种农药残留量

目的 建立大豆中有机磷、有机氯及拟除虫菊酯三类53种常见农药的气质联用定量测定法。方法 采用快速溶剂萃取仪提取,经PSA及C18粉末净化,在线凝胶渗透色谱串联气质联用法测定。结果 该方法在0.010~0.500 mg/L 范围内有良好的线性关系, 相关系数r2＞0.990, 方法平均回收率范围为60.0%~120%,相对标准偏差为2.0 ~15.0%；测定低限为0. 010 mg/kg。结论 此方法灵敏度高、准确、重现性好, 适用于大豆中有机磷、有机氯及拟除虫菊酯三类53种常见农药的检测。

Determination of 53 pesticide residues in soybeans by gas chromatography- tandem mass spectrometry with ASE-gel permeation chromatography

Objective To develop a gas chromatography-tandem mass spectrometry method for the simultaneous determination of 53 organophosphate, organochlorine and pyrethroids pesticide residues in soybeans. Methods Homogenized samples were extracted with accelerated solvent extractor (ASE), purified by primary secondary amine (PSA) and C18 powder, and determined by on-line gel permeation chromatogra-phy-tandem gas chromatograph-mass spectrometer (GPC-GC/MS) system. Results The calibration curves of 53 pesticide residues were linear in the range of 0.01~0.50 mg/L with a good correlation, with coefficients more than 0.990. The recoveries of the method ranged from 60% to 120%. And the relative standard deviations were 2%~15%. The limits of quantification were 0.01 mg/kg. Conclusion This method is sensitive, accurate, and reliable, which is suitable for the determination and confirmation of 53 organophosphate, organochlorine and pyrethroids pesticide residues in soybeans.