气相色谱-负化学源-串联质谱法测定动物源食品中氟虫腈及其4 种代谢产物残留量

doi:10.7506/spkx1002-6630-20200302-028

食品科学 ›› 2020, Vol. 41 ›› Issue (16): 327-331.doi: 10.7506/spkx1002-6630-20200302-028

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气相色谱-负化学源-串联质谱法测定动物源食品中氟虫腈及其4 种代谢产物残留量

韩超，胡贝贞，金娜，刘滨，沈燕，金建昌，陈树兵,

（1.浙江树人大学生物与环境工程学院，浙江杭州 310015；2.绍兴海关综合技术服务中心，浙江绍兴 312000；3.温州海关综合技术服务中心，浙江温州 325027；4.宁波海关技术中心，浙江宁波 315040）

发布日期:2020-08-19
基金资助:
浙江树人大学科研启动费项目（2019R024）

Determination of Fipronil and Four Metabolites in Animal-Derived Foods by Gas Chromatography-Negative Chemical Ionization-Tandem Mass Spectrometry

HAN Chao, HU Beizhen, JIN Na, LIU Bin, SHEN Yan, JIN Jianchang, CHEN Shubing,

(1. College of Biology and Environmental Engineering, Zhejiang Shuren University, Hangzhou 310015, China;2. Comprehensive Technical Service Center of Shaoxing Customs, Shaoxing 312000, China;3. Comprehensive Technical Service Center of Wenzhou Customs, Wenzhou 325027, China;4. Technology Center of Ningbo Customs, Ningbo 315040, China)

Published:2020-08-19

摘要/Abstract

摘要： 建立动物源食品（鸡蛋、鸡肉、鸡肝）中氟虫腈及其4 种代谢产物（氟甲腈、氟虫腈砜、氟虫腈硫醚、酰胺氟虫腈）残留量的气相色谱-负化学源-串联质谱（gas chromatography-negative chemical ionization-tandem mass spectrometry，GC-NCI-MS/MS）测定方法。样品经乙腈（正己烷饱和）提取后，采用改进的QuEChERS净化和GC-NCI-MS/MS的多反应监测模式检测，基质匹配工作曲线法定量。实验结果表明，氟虫腈及其4 种代谢产物在1～100 μg/L质量浓度范围内线性良好，线性系数均大于0.999 0，氟甲腈、氟虫腈和氟虫腈硫醚定量限（RSN≥10）为0.5 μg/kg，氟虫腈砜和酰胺氟虫腈定量限为1.0 μg/kg。在2.0、10.0、20.0 μg/kg加标水平下，回收率在80.2%～108.7%之间，相对标准偏差为3.8%～10.2%。该方法灵敏度高、准确性好，能够满足动物源食品中氟虫腈及其4 种代谢产物残留量的测定。

关键词: 动物源食品；氟虫腈；代谢产物；气相色谱-负化学源-串联质谱

Abstract: A gas chromatography-negative chemical ionization-tandem mass spectrometry (GC-NCI-MS/MS) method for the determination of the residues of fipronil and its four metabolites (fipronil desulfinyl, fipronil sulfone, fipronil sulfide, and fipronil carboxamide) in animal-derived foods (egg, chicken, and chicken liver) was established. The samples were extracted with acetonitrile (saturated with n-hexane), and the extract was cleaned up using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method before being detected by GC-NCI-MS/MS in the multi-reaction monitoring (MRM) mode. The matrix matched standard curve method was used for quantitation. Results showed that there was a good linearity for all analytes in the range of 1–100 μg/L with correlation coefficient (r2) higher than 0.999 0. The limit of quantitation (LOQ, RSN ≥ 10) of the method was 0.5 μg/kg for fipronil disulfonyl, fipronil, fipronil sulfide and 1.0 μg/kg for fipronil sulfone and fipronil carboxamide. The average recoveries at three spiked concentration levels (2.0, 10.0, and 20.0 μg/kg) were 80.2%–108.7% with relative standard deviations (RSDs) of 3.8%–10.2%. This method exhibited high sensitivity and accuracy, and could be used for the determination of the residues of fipronil and its four metabolites in animal-derived foods.

Key words: animal-derived foods; fipronil; metabolites; gas chromatography-negative chemical ionization-tandem mass spectrometry

中图分类号:

TS207.3

韩超，胡贝贞，金娜，刘滨，沈燕，金建昌，陈树兵,. 气相色谱-负化学源-串联质谱法测定动物源食品中氟虫腈及其4 种代谢产物残留量[J]. 食品科学, 2020, 41(16): 327-331.

HAN Chao, HU Beizhen, JIN Na, LIU Bin, SHEN Yan, JIN Jianchang, CHEN Shubing,. Determination of Fipronil and Four Metabolites in Animal-Derived Foods by Gas Chromatography-Negative Chemical Ionization-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2020, 41(16): 327-331.

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气相色谱-负化学源-串联质谱法测定动物源食品中氟虫腈及其4 种代谢产物残留量

Determination of Fipronil and Four Metabolites in Animal-Derived Foods by Gas Chromatography-Negative Chemical Ionization-Tandem Mass Spectrometry

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