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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1,胡贝贞2,朱振瓯3,刘滨3,沈燕1,金建昌1,陈树兵4   

  1. 1. 浙江树人大学
    2. 绍兴海关综合技术服务中心
    3. 温州海关综合技术服务中心
    4. 宁波检验检疫局检验检疫技术中心
  • 收稿日期:2020-03-02 修回日期:2020-06-15 出版日期:2020-08-25 发布日期:2020-08-19
  • 通讯作者: 陈树兵 E-mail:shubingchen@126.com
  • 基金资助:
    浙江树人大学科研启动费

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

2, 2, 2, 2, 2,Shu-bing CHENG   

  • Received:2020-03-02 Revised:2020-06-15 Online:2020-08-25 Published:2020-08-19
  • Contact: Shu-bing CHENG E-mail:shubingchen@126.com

摘要: 建立了动物源食品(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(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(MRM)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-1浓度范围内线性良好,线性系数均大于0.9990,定量限(LOQ,S/N≥10)氟甲腈、氟虫腈和氟虫腈硫醚为0.5μg kg-1,氟虫腈砜和酰胺氟虫腈为1.0 μg kg-1。在2.0、5.0、10.0 μg kg-1加标水平下,回收率在80.2~108.7 %之间,相对标准偏差为4.1~10.2 %。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-串联质谱法

Abstract: A gas chromatography-negative chemical ionization-tandem mass spectrometry (GC-NCI-MS/MS) method for the determination of fipronil and four metabolites residues(fipronil desulfinyl, fipronil, fipronil sulfide, fipronil, fipronil sulfide and fipronil carboxamide) in animal-derived foods (egg, chicken, chicken liver) was established. The samples were extracted with acetonitrile (saturated with n-hexane), using QuEChERS purification and GC-NCI-MS/MS multi-response monitoring (MRM) mode detection, matrix matched standard curve method was selected for quantitation. Results showed that there was a good linearity for fipronil and four metabolites in the range of 1~100 μg/L with correlation coefficient (r2) higher than 0.9990. The limit of quantitation (LOQ, S/N≥10) of the method was 0.5 for fipronil desulfinyl, fipronil, fipronil sulfide and 1.0 μg kg-1for fipronil sulfone, fipronil carboxamide. The average recoveries at three spiking levels (2.0, 5.0, 10.0 μg kg-1) were 80.2~108.7 %. Relative standard deviation (RSD) were 4.1~10.2 %, which is indicative of the good recovery and precision of the method. This method has high sensitivity and accuracy, and can be used for the determination of fipronil and four metabolites residues in animal-derived foods.

Key words: animal-derived foods, fipronil, metabolites, gas chromatography-negative chemical ionization-tandem mass spectrometry (GC-NCI-MS/MS)

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