Determination of 17 Neonicotinoid Pesticides and Their Metabolites in Baby Fruit and Vegetable Rice Flour by High Performance Liquid Chromatography－Tandem Mass Spectrometry

GUO Li-qiang; LIU Yong-qiang; WANG Le; LI Kai; XU Xiao-jie

doi:10.19969/j.fxcsxb.22060103

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Determination of 17 Neonicotinoid Pesticides and Their Metabolites in Baby Fruit and Vegetable Rice Flour by High Performance Liquid Chromatography－Tandem Mass Spectrometry

Special Column for DRE Thesis Competition | 更新时间：2023-01-04

- Determination of 17 Neonicotinoid Pesticides and Their Metabolites in Baby Fruit and Vegetable Rice Flour by High Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 41, Issue 12, Pages: 1773-1778(2022)
- 作者机构：
  
  1.潍坊海关，山东潍坊 261041
  2.济南海关技术中心，山东济南 250014
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22060103
  CLC：
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郭礼强,刘永强,王乐等.HPLC－MS/MS法测定婴幼儿果蔬米粉中17种新烟碱类杀虫剂及代谢物[J].分析测试学报,2022,41(12):1773-1778.

GUO Li-qiang,LIU Yong-qiang,WANG Le,et al.Determination of 17 Neonicotinoid Pesticides and Their Metabolites in Baby Fruit and Vegetable Rice Flour by High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(12):1773-1778.
郭礼强,刘永强,王乐等.HPLC－MS/MS法测定婴幼儿果蔬米粉中17种新烟碱类杀虫剂及代谢物[J].分析测试学报,2022,41(12):1773-1778. DOI： 10.19969/j.fxcsxb.22060103.

GUO Li-qiang,LIU Yong-qiang,WANG Le,et al.Determination of 17 Neonicotinoid Pesticides and Their Metabolites in Baby Fruit and Vegetable Rice Flour by High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(12):1773-1778. DOI： 10.19969/j.fxcsxb.22060103.

摘要

建立了婴幼儿果蔬米粉中17种新烟碱类杀虫剂及代谢物的高效液相色谱－串联质谱（HPLC－MS/MS）分析方法。样品经含1%（体积分数）甲酸的乙腈提取，QuEChERS净化，氮气吹干后，用含0.1%甲酸的乙腈水溶液（1∶4，体积比）定容。采用Acquity BEH C,18,色谱柱（2.1 mm × 100 mm，1.7 μm）分离，0.1%甲酸水溶液和乙腈作为流动相梯度洗脱，高效液相色谱－串联质谱检测。结果表明，17种目标物在对应的质量浓度范围内线性良好，相关系数（,r,）均大于0.995 4；方法检出限（LOD）为0.02 ~ 0.15 μg/kg，定量下限（LOQ）为0.06 ~ 0.50 μg/kg；在LOQ、2.0 μg/kg、10.0 μg/kg 3个加标水平下，17种目标物在水果米粉中的平均回收率为62.5% ~ 103%，相对标准偏差（RSD）为3.5% ~ 17%；蔬菜米粉中的平均回收率为66.4% ~ 108%，RSD为4.3% ~ 13%。该方法灵敏、准确，简便、可靠，适用于婴幼儿果蔬米粉中17种新烟碱类杀虫剂及代谢物的同时检测。

Abstract

A high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） was developed for the simultaneous determination of 17 neonicotinoid pesticides and their metabolites in baby fruit and vegetable rice flour．After moistened with water，the samples were added anhydrous magnesium sulfate（MgSO,4,），then extracted with acetonitrile solution containing 1%（volume fraction） formic acid，followed by QuEChERS purification．The final extracts were dried under nitrogen，and the residues were dissolved in water－acetonitrile containing 0.1% formic acid（4∶1，volume ratio），then separated on an Acquity BEH C,18,（2.1 mm × 100 mm，1.7 μm） column by gradient elution with water containing 0.1% formic acid and acetonitrile as mobile phases．The analytes were finally detected by HPLC－MS/MS in positive electrospray ionization（ESI,+,） mode under multiple reaction monitoring（MRM） mode，and quantified by the external standard calibration curve method．Under the optimal conditions，17 analytes were well separated within 10 min．The calibration curves for 17 analytes were linear in the respective mass concentration ranges with their correlation coefficients（,r,） larger than 0.995 4．The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.02－0.15 μg/kg and 0.06－0.50 μg/kg，respectively．The average recoveries for 17 analytes in baby fruit rice flour samples at three spiked levels of LOQ level，2.0 μg/kg and 10.0 μg/kg ranged from 62.5% to 103%，with relative standard deviations（RSDs） of 3.5%－17%，while the average recoveries for vegetable rice flour samples at three spiked levels ranged from 66.4% to 108%，with RSDs of 4.3%－13%．The established method was applied to the detection of 17 neonicotinoid pesticides and their metabolites in baby fruit and vegetable rice flour samples by random sampling principle，and acetamiprid was detected in one of the vegetable rice flour samples with content of 7.4 µg/kg．The method was sensitive，accurate，convenient and reliable，and it could meet the requirements for simultaneous detection of 17 neonicotinoid pesticides and their metabolites in baby fruit and vegetable rice flour.

关键词

婴幼儿米粉高效液相色谱－串联质谱（HPLC－MS/MS）新烟碱类杀虫剂代谢物

Keywords

baby rice flourhigh performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）neonicotinoid pesticidesmetabolites

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Pearl River Fisheries Research Institute，Chinese Academy of Fishery Sciences/Laboratory of Aquatic Product Quality and Safety Risk Assessment，Ministry of Agriculture and Rural Affairs（Guangzhou）/Key Laboratory of Aquatic Animal Immune Technology of Guangdong Province

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