色谱

色谱 ›› 2017, Vol. 35 ›› Issue (12): 1224-1228.DOI: 10.3724/SP.J.1123.2017.09033

• 特别策划:“毒鸡蛋”检测专栏 • 上一篇    下一篇

气相色谱-负化学源质谱法测定禽蛋及蛋制品中氟虫腈及其代谢物

沈伟健, 柳菡, 张睿, 余可垚, 蔡理胜, 刘艳, 王红   

  1. 江苏出入境检验检疫局食品实验室, 江苏 南京 210019
  • 收稿日期:2017-09-19 出版日期:2017-12-08 发布日期:2017-12-15
  • 通讯作者: 沈伟健,Tel:(025)52345193,E-mail:shenwj18@jsciq.gov.cn
  • 基金资助:

    国家认证认可监督管理委员会行业标准紧急制定任务（2017B261j）.

Determination of fipronil and its metabolites in eggs and egg products with gas chromatography-negative chemical ionization-mass spectrometry

SHEN Weijian, LIU Han, ZHANG Rui, YU Keyao, CAI Lisheng, LIU Yan, WANG Hong   

  1. Food Laboratory of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210019, China
  • Received:2017-09-19 Online:2017-12-08 Published:2017-12-15
  • Supported by:

    Industrial Standard of Urgent Tasks Issued by National Certification and Accreditation Regulatory Commission (No. 2017B261j).

PDF

321

被引次数

5

摘要：

建立了气相色谱-负化学源质谱联用技术（GC-NCI-MS）测定禽蛋及蛋制品中氟虫腈及其3种代谢物残留量的方法。样品经乙腈提取，分散固相萃取技术QuEChERS净化，采用基质校正曲线外标法定量。在0.005~0.10 mg/L范围内氟虫腈及其3种代谢物均呈现良好的线性关系，所有目标物的定量限均在0.025~0.10 μg/kg范围内，均能满足国内外的限量要求。在0.1、2.0、4.0、20.0 μg/kg4个添加水平下，氟虫腈及其3种代谢物的平均回收率均处于87.0%~99.3%，RSD均≤ 12.7%，说明该法有较高的准确度和较好的稳定性。综上所述，该法灵敏度、准确度较高，精密度较好，可用于禽蛋及蛋制品中氟虫腈及其代谢物残留量的测定。

关键词: QuEChERS, 蛋制品, 氟虫腈及其代谢物, 负化学源, 气相色谱-质谱, 禽蛋

Abstract:

A method was established for the determination of fipronil and its metabolites in eggs and egg products with gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). The targets were extracted from samples with acetonitrile, and followed by a simple cleanup step known as dispersive solid-phase extraction QuEChERS. The extracts were determined by GC-NCI-MS, and quantified by external standard method with matrix correction standard curves. The recoveries were in the range of 87.0% to 99.3% at four spiked levels (0.1, 2.0, 4.0 and 20.0 μg/kg), and all RSDs were not more than 12.7% for the four analytes. The linearity of the method was good between 0.005 and 0.10 mg/L, and all LOQs were less than 0.10 μg/kg. So this method can be used to determine the residues of fipronil and its metabolites in eggs and egg products

Key words: egg products, eggs, fipronil and its metabolites, gas chromatography-mass spectrometry (GC-MS), negative chemical ionization (NCI), QuEChERS

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