食品科学 ›› 2013, Vol. 34 ›› Issue (10): 272-275.doi: 10.7506/spkx1002-6630-201310060

• 分析检测 • 上一篇    下一篇

液相色谱-串联质谱法测定动物源性食品中氯虫苯甲酰胺和氟虫酰胺残留量

张 云,郑敬峰,李耀平,许彩霞,侯 杰   

  1. 1.三明出入境检验检疫局,福建 三明 365000; 2.福建出入境检验检疫局,福建 福州 350003
  • 收稿日期:2012-01-21 修回日期:2013-04-09 出版日期:2013-05-25 发布日期:2013-05-07
  • 通讯作者: 张云 E-mail:48965461@qq.com
  • 基金资助:

    福建检验检疫局科技项目

LC-MS/MS Determination of Chloranteraniliprole and Flubendiamide Residues in Animal-Derived Foodstuffs

ZHANG Yun,ZHENG Jing-feng,LI Yao-ping,XU Cai-xia,HOU Jie   

  1. 1. Sanming Entry-Exit Inspection and Quarantine Bureau, Sanming 365000, China;
    2. Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350003, China
  • Received:2012-01-21 Revised:2013-04-09 Online:2013-05-25 Published:2013-05-07

摘要:

建立动物源性食品中氯虫苯甲酰胺和氟虫酰胺残留量的液相色谱-串联质谱(LC-MS/MS)测定方法。动物源性食品中的氯虫苯甲酰胺和氟虫酰胺,经乙腈和乙酸铵混合提取液提取后,过中性氧化铝柱净化,以乙腈-5mmol/L乙酸铵-甲酸(70:30:0.1,V/V)作为流动相,LC-MS/MS电喷雾电离源,正离子多反应检测模式测定,外标法定量。测定结果表明:采用本方法检测氯虫苯甲酰胺和氟虫酰胺,检出限均可达到1μg/kg,质量浓度在1~250μg/L之间线性关系良好,相关系数均大于0.999,对于1、2、10μg/kg水平添加回收率范围在73.5%~101.2%之间;相对标准偏差范围在3.72%~11.05%之间。

关键词: 动物源性食品, 氯虫苯甲酰胺, 氟虫酰胺, 液相色谱-串联质谱, 测定

Abstract:

A method for the determination chloranteraniliprole and flubendiamide residues in animal-origin foodstuffs
using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. Residues of chloranteraniliprole
and flubendiamide in animal-origin foodstuffs were extracted with a mixture of acetonitrile and ammonium acetate and
decontaminated on a neutral alumina column using acetonitrile and aqueous solution containing 5 mmol/L ammonium
acetate (70:30) as mobile phase. LC-MS/MS analysis of the analytes was conducted by electrospray ionization (ESI) in a
positive mode using multiple reaction monitoring, and quantified by an external standard method. The results showed that the
detection limit was 1 μg/kg for both chloranteraniliprole and flubendiamide. An excellent linear relationship was observed in the
range of 1 to 250 μg/L with a relative standard deviation of 0.999. The recovery rates of chloranteraniliprole and flubendiamide
at spiked levels of 1, 2 μg/kg and 10 μg/kg were 73.5%–101.2% with relative standard deviation of 3.72%–11.05%.

Key words: animal-origin foodstuffs, chloranteraniliprole, flubendiamide, liquid chromatography-tandem mass spectrometry (LC-MS/MS), determination

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