食品科学

• 分析检测 • 上一篇    下一篇

液相色谱-质谱同时测定水产品中78 种兽药残留

李仲超1,2   

  1. 1.厦门市产品质量监督检验院,福建 厦门 361004;2.厦门市工业产品生产许可证审查技术中心,福建 厦门 361004
  • 出版日期:2014-08-25 发布日期:2014-08-25

Simultaneous Determination of Veterinary Drug Residues in Aquatic Products by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS-MS)

LI Zhong-chao1,2   

  1. 1. Xiamen Products Quality Supervision and Inspection Institute, Xiamen 361004, China;
    2. Xiamen Industrial Products Production License Review Technology Center, Xiamen 361004, China
  • Online:2014-08-25 Published:2014-08-25

摘要:

运用液相色谱-质谱技术建立水产品(鱼、虾和贝)中78 种兽药的同时测定方法。含0.1%甲酸的乙腈溶液进行提取,考察不同萃取溶剂及Na2EDTA添加量对目标兽药回收率影响。目标兽药在0.1~100 μg/kg范围内线性良好;以基底匹配工作曲线和替代物法分别进行定量和质控,4 μg/kg和20 μg/kg两个加标量条件下鱼、虾、贝肉的加标回收率和相对标准偏差(n=4)分别为40.8%~125.6%和0.1%~16.0%(鱼)、42.9%~131.9%和0.1%~14.0%(虾)、及43.5%~136.4%和0.3%~15.8%(贝),方法检测限为0.1~0.5 μg/kg。方法灵敏、准确、快速,可应用于福建漳州养殖区虾样兽药污染情况调查。

关键词: 液相色谱-质谱, 同时测定, 水产品, 兽药

Abstract:

A method for the simultaneous determination of 78 veterinary drugs in aquatic products (fish, shrimp and
shellfish) was established using liquid chromatography tandem mass spectrometry (LC-MS-MS). Effects of experimental
conditions such as extraction solvents and Na2EDTA adding on extraction efficiency were investigated. Under the optimized
conditions, recoveries of 78 target drugs calculated from matrix match calibration curve at spiked level of 4 and 20 μg/kg
were 40.8%–125.6% for fish, 42.9%–131.9% for shrimp and 43.5%–136.4% for shellfish with RSD (n = 4) of 0.1%–16.0%,
0.1%–14.0% and 0.3%–15.8%, respectively. The detection limits drugs ranged from 0.1 to 0.5 μg/kg. The method is
sensitive, accurate and fast and can be successfully applied in the analysis of residual veterinary drugs in shrimp samples
from the aquatic farming areas of Zhangzhou, Fujian province.

Key words: liquid chromatography tandem mass spectrometry (LC-MS-MS), simultaneous determination, aquatic products, veterinary drugs

中图分类号: