Screening of 33 Neonicotinoid Insecticides and Fungicides in Tropical Fruits by Liquid Chromatography－High Resolution Mass Spectrometry with a Modified QuEChERS Method

MEN Xue; WU Xing-qiang; TONG Kai-xuan; XIE Yu-jie; LI Bei; LI Jian-xun; WEI Jing; WANG Yong-li; FAN Chun-lin; CHEN Hui

doi:10.19969/j.fxcsxb.22041202

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Screening of 33 Neonicotinoid Insecticides and Fungicides in Tropical Fruits by Liquid Chromatography－High Resolution Mass Spectrometry with a Modified QuEChERS Method

Scientific Papers | 更新时间：2022-06-22

- Screening of 33 Neonicotinoid Insecticides and Fungicides in Tropical Fruits by Liquid Chromatography－High Resolution Mass Spectrometry with a Modified QuEChERS Method
- Journal of Instrumental Analysis Vol. 41, Issue 6, Pages: 820-826(2022)
- 作者机构：
  
  1.中国检验检疫科学研究院国家市场监管重点实验室（食品质量与安全），北京 100176
  2.山东农业大学食品科学与工程学院，山东泰安 271018
  3.海南省食品检验检测中心国家市场监管重点实验室（热带果蔬质量与安全），海南海口 570314
  4.中国农业科学院农产品加工研究所，北京 100193
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22041202
  CLC：
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门雪,吴兴强,仝凯旋等.改进的QuEChERS法结合液相色谱－高分辨质谱筛查热带水果中33种新烟碱类杀虫剂及杀菌剂[J].分析测试学报,2022,41(06):820-826.

MEN Xue,WU Xing-qiang,TONG Kai-xuan,et al.Screening of 33 Neonicotinoid Insecticides and Fungicides in Tropical Fruits by Liquid Chromatography－High Resolution Mass Spectrometry with a Modified QuEChERS Method[J].Journal of Instrumental Analysis,2022,41(06):820-826.
门雪,吴兴强,仝凯旋等.改进的QuEChERS法结合液相色谱－高分辨质谱筛查热带水果中33种新烟碱类杀虫剂及杀菌剂[J].分析测试学报,2022,41(06):820-826. DOI： 10.19969/j.fxcsxb.22041202.

MEN Xue,WU Xing-qiang,TONG Kai-xuan,et al.Screening of 33 Neonicotinoid Insecticides and Fungicides in Tropical Fruits by Liquid Chromatography－High Resolution Mass Spectrometry with a Modified QuEChERS Method[J].Journal of Instrumental Analysis,2022,41(06):820-826. DOI： 10.19969/j.fxcsxb.22041202.

摘要

该文采用改进的QuEChERS法结合液相色谱－四极杆－飞行时间质谱（LC－Q－TOF MS）建立了一种检测4种热带水果（芒果、香蕉、释迦和莲雾）中33种农药（包括8种新烟碱类杀虫剂、25种杀菌剂）残留的分析方法。比较萃取溶剂体积、萃取盐种类以及净化剂种类和用量对样品提取与净化的影响。在最优条件下，采用LC－Q－TOF MS对样品进行检测，基质匹配外标法定量分析。该方法可有效降低基质效应，33种农药在各自线性范围内线性关系良好，相关系数（,r,2,）均大于0.99。4种热带水果的筛查限（SDL）为0.5～20 µg/kg，定量下限（LOQ）为0.5～50 µg/kg。方法的准确度与精密度通过芒果基质的加标回收实验进行验证，在1、2、10倍定量下限的加标水平下，33种农药的回收率为70.5%～116%，相对标准偏差（RSD，,n ,= 5）均不大于20%。方法成功用于102批热带水果实际样品的筛查。该方法具有前处理操作简单、快速、灵敏的特点，适用于热带水果中新烟碱类杀虫剂及杀菌剂残留的检测。

Abstract

A liquid chromatography－quadrupole-time-of-flight mass spectrometry（LC－Q－TOF MS） with a modified QuEChERS method was developed for the detection of 33 pesticide residues，including 8 neonicotinoid insecticides and 25 fungicides in four tropical fruits（mango，banana，sweetsop and wax apple）．The pretreatment parameters were optimized by comparing the spiked recoveries obtained with different extraction solvent volumes，buffer salts，and clean-up adsorbent types．Under the optimal experimental conditions，the tropical fruit samples were extracted with 1% acetonitrile acetate in buffer salts（EN salts），and subsequently purified in 15 mL tubes of 900 mg MgSO,4,，150 mg PSA，50 mg C,18, and 15 mg GCB．The sample solutions were detected by LC－Q－TOF MS in positive ion mode under all-ion fragmentation acquisition mode（All Ions MS/MS），and quantified by the matrix-matched external standard method．The method could effectively reduce the matrix effect．Under the optimized conditions，the 33 pesticides showed good linearity in their respective linear ranges，with their correlation coefficients（,r,2,） more than 0.99．The screening detection limits（SDLs） for four tropical fruits were in the range of 0.5－20 µg/kg，and the limits of quantitation（LOQs） were in the range of 0.5－50 µg/kg．The accuracy and precision of the method were verified by the spiked recovery experiments for mangoes．The recoveries for 33 pesticides at three spiked levels ranged from 70.5% to 116%，with relative standard deviations（RSDs） no more than 20%．Meanwhile，the method was successfully applied to the detection of 102 commercial tropical fruits samples．Characterized with simplicity，rapidness and sensitivity，the method was suitable for the detection of neonicotinoid pesticide and fungicide residues in tropical fruits．

关键词

热带水果液相色谱－四极杆－飞行时间质谱（LC－Q－TOF MS）QuEChERS新烟碱类杀虫剂杀菌剂

Keywords

tropical fruitsliquid chromatography－quadrupole-time-of-flight mass spectrometry （LC－Q－TOF MS）QuEChERSneonicotinoid insecticidesfungicides

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Related Institution

College of Horticulture and Landscape，Tianjin Agricultural University

Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables；Key Laboratory of Quality and Safety Control for Subtropical Fruit and Vegetable，Ministry of Agriculture and Rural Affairs；Analysis and Test Center，Chinese Academy of Tropical Agricultural Sciences

Tea Research Institute，Chinese Academy of Agricultural Sciences

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