QuEChERS-液相色谱-串联质谱法同时测定蔬菜中7种新烟碱类农药

Simultaneous determination of 7 neonicotinoid pesticides in vegetables by QuEChERS-liquid chromatography-tandem mass spectrometry

王秀丽 ¹张梅超 ¹倪瑞敏 ¹管淑霞 ¹张玉洁¹

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作者信息

1. 威海市食品药品检验检测研究院威海市食品药品质量评价与技术研究重点实验室,山东威海 264200
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摘要

[目的]建立一种同时测定蔬菜中7种新烟碱类农药残留量的分析方法.[方法]样品采用1％酸化乙腈提取,QuEChERS前处理方法,结合液相色谱-串联质谱法(LC-MS/MS)进行定性定量测定.[结果]7种新烟碱类农药在0.5～20.0 μg/L质量浓度范围内呈良好的线性关系,相关系数r的范围为0.998 96～0.999 92,方法检出限(LOD)和定量限(LOQ)分别为1.0、2.0μg/kg.在韭菜、黄瓜、芹菜3种基质中,进行1、2、10μg/kg3个水平的加标试验,平均回收率为70.6％～122.6％,相对标准偏差(RSD)为2.0％～8.8％.[结论]该方法操作简单快捷,具有较高的灵敏度、准确度和精密度,且可同时测定多种新烟碱类农药,适用于批量蔬菜样品的测定,具有较高的实际应用意义.

Abstract

[Aims]Establishing an analytical method for simultaneous determination of 7 neonicotinoid pesticides residues in vegetables.[Methods]The samples were extracted by 1％acidified acetonitrile,pre-treated by QuEChERS,and qualitatively and quantitatively determined by LC-MS/MS.[Results]The seven neonicotinoid pesticides showed a good linear relationship in the concentration range from 0.5 to 20.0 μg/L,the correlation coefficient r ranged from 0.998 96 to 0.999 92.The limit of detection(LOD)was 1.0 pg/kg and the limit of quantification(LOQ)was 2.0 pg/kg.The average recovery was 70.6％-122.6％and the relative standard deviation(RSD)was 2.0％-8.8％at 3 spiked levels of 1,2 and 10 pg/kg in leek,cucumber and celery substrates.[Conclusions]The method is simple and fast in operation,has high sensitivity,accuracy and precision,and can simultaneously determine a variety of neonicotinoid pesticides.It is suitable for the determination of batch vegetable samples,and has high practical significance.

关键词

液相色谱-串联质谱/新烟碱类农药/QuEChERS

Key words

liquid chromatography-tandem mass spectrometry/neonicotinoid pesticide/QuEChERS

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出版年

2024

农药

沈阳化工研究院有限公司

农药

CSTPCD北大核心

影响因子：0.665

ISSN：1006-0413

参考文献量25

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