气相色谱-串联质谱测定水稻中10种拟除虫菊酯类杀虫剂农药残留

Determination of 10 Pyrethroids Pesticide Residues in Rice by GC-MS-MS

[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,弗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时(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] A method was developed for the determination of 10 pymthroids pesticide residues in rice by GC-MS-MS. [ Method ] Pyrethroids were extracted with acetonitrile, followed by a salting-out step with anhydrous magnesium sulfate and sodium chloride, cleaned up by florisil solid phase extraction （SPE） cartridge, and determined by multiple reaction monitoring mode. [ Result ] The method showed good linearity over the range of 0.010 - 0. 500 mg/L for 10 pyrethroids pesticide with correlation coefficients over 0.99. The detection limits were 0. 005 - 0. 010 mg/kg. The method was validated by analyzing samples spiked with 0.05,0.10, 0.20 mg/kg of 10 pyrethroids pesticide, re- spectively. The average recoveries in rice ranged from 75.0% -115.5 % , and the relative standard deviations （RSD）were between 3.9% - 6.9%. [ Conclusion] The method is easy, accuracy and reliable, which can meet the requirement for the simultaneous determination and con- firmation of pyrethroids pesticide residues in rice.