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

doi:10.3724/SP.J.1123.2016.05009

色谱 ›› 2016, Vol. 34 ›› Issue (9): 880-887.DOI: 10.3724/SP.J.1123.2016.05009

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

陈建波, 马琳, 黄兰淇, 吴爱娟, 占绣萍, 赵莉

上海市农业技术推广服务中心, 上海 201103

收稿日期:2016-05-12 出版日期:2016-09-08 发布日期:2016-08-26
通讯作者: 赵莉
基金资助:
上海市农委科技攻关项目（2015-4-6）.

Rapid screening of illegally added insecticides in pesticide formulations by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry

CHEN Jianbo, MA Lin, HUANG Lanqi, WU Aijuan, ZHAN Xiuping, ZHAO Li

Shanghai Agriculture Technical Extension Service Center, Shanghai 201103, China

Received:2016-05-12 Online:2016-09-08 Published:2016-08-26
Supported by:
Shanghai Agricultural Committee Projects for Science and Technology (No. 2015-4-6).

摘要/Abstract

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（R²）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。

关键词: 超高效液相色谱-四极杆-飞行时间质谱, 快速筛查, 农药制剂, 杀虫剂

Abstract:

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.

Key words: insecticide, pesticide formulations, rapid screening, ultra performance liquid chromatography-quadruple-time of flight mass spectrometry (UPLC-Q-TOF MS)

中图分类号:

O658

陈建波, 马琳, 黄兰淇, 吴爱娟, 占绣萍, 赵莉. 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[J]. 色谱, 2016, 34(9): 880-887.

CHEN Jianbo, MA Lin, HUANG Lanqi, WU Aijuan, ZHAN Xiuping, ZHAO Li. Rapid screening of illegally added insecticides in pesticide formulations by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(9): 880-887.

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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

Rapid screening of illegally added insecticides in pesticide formulations by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry

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