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[目的]建立水稻中10种拟除虫菊酯类杀虫剂农药残留气相色谱-串联质谱测定方法。[方法]将样品用乙腈提取,采用无水硫酸镁、氯化钠盐析,佛罗里硅土柱萃取净化进行前处理,采用多反应监测模式测定。[结果]浓度为0.010~0.500 mg/L范围内与峰面积呈线性关系,相关系数均大于0.99,最低检测限在0.005~0.010 mg/kg。当添加水平为0.05、0.10、0.20 mg/kg(n=5),回收率为75.0%~115.5%,相对标准偏差为3.9%~6.9%。[结论]该方法简便、准确、可靠,能同时定性和定量,可用于水稻中拟除虫菊酯类杀虫剂农药残留的快速检测与确证。
[Objective] The research aimed to establish a method for the determination of pesticide residues in 10 pyrethroid pesticides in rice by gas chromatography-tandem mass spectrometry. [Method] The sample was extracted with acetonitrile, pretreated with anhydrous magnesium sulfate, salted-sodium chloride and Florisil silica column, and determined by multi-reaction monitoring mode. [Result] The linear relationship was obtained between the concentration and peak area in the range of 0.010-0.500 mg / L, the correlation coefficients were both above 0.99 and the lowest detection limit was between 0.005 and 0.010 mg / kg. The recoveries ranged from 75.0% to 115.5% at 0.05, 0.10 and 0.20 mg / kg (n = 5) with relative standard deviations of 3.9% to 6.9%. [Conclusion] The method was simple, accurate and reliable and could be qualitatively and quantitatively determined at the same time. It could be used for rapid detection and confirmation of pyrethroid pesticide residues in rice.