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超高效液相色谱-四极杆-飞行时间质谱法快速筛查农药制剂中非法添加的杀虫剂 被引量:14

Rapid screening of illegally added insecticides in pesticide formulations by ultra performance liquid chromatographyquadrupole-time of flight mass spectrometry
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摘要 建立了农药制剂中48种非法添加杀虫剂的超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF MS)快速 筛查方法.可湿性粉剂、乳油和悬浮剂3种剂型的农药制剂样品经甲醇溶解、提取后,采用UPLC-Q-TOF MS检测, 48种杀虫剂在0. 5-20 mg/L范围内线性关系良好,线性相关系数(五2)大于0. 99.48种农药的定量限为0. 05-0.4 mg/kg,检出限为0.01-0.2 mg/kg,低、中、高3个加标水平下的平均回收率为86.3 % -101 . 5 %,相对标准偏差 为1.7%-4.0%.该方法快速、准确,可用于农药制剂中多种杀虫剂的快速筛查. An analytical method was established for the rapid screening of 48 illegally added insecticides in pesticide formulations by ultra performance liquid chromatography-quadrupole- time of flight mass spectrometry (UPLC-Q-TOF MS). Three pesticide formulations of wettable powder,emulsifiable concentrate,suspension concentrate were extracted with methanol,then detected by UPLC-Q-TOF MS. The calibration curves were linear in the range of 0. 5-20 mg/L with the correlation coefficients more than 0. 99 for the 48 insecticides. The limits of quantification (LOQs) were 0. 05-0. 4 mg/kg. The limits of detection (LODs) were 0. 01-0. 2 mg/kg. The added recoveries for all the insecticides were 86. 3% -101. 5 % with the relative standard deviations ranging from 1.7% to 4.0%. This method has the characteristics of rapid and accurate screening,which can meet the requirement of the determination of the 48 insecticides in pesticide formulations.
出处 《色谱》 CAS CSCD 北大核心 2016年第9期880-887,共8页 Chinese Journal of Chromatography
基金 上海市农委科技攻关项目(2015-4-6)~~
关键词 超高效液相色谱-四极杆-飞行时间质谱 快速筛查 杀虫剂 农药制剂 ultra performance liquid chromatography-quadruple-time of flight mass spectrometry (UPLC-Q-TOF MS) rapid screening pesticide formulations insecticide
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