超高效液相色谱串联质谱法同时测定水产品中6种兽药残留

doi:10.7506/spkx1002-6630-201110048

食品科学 ›› 2011, Vol. 32 ›› Issue (10): 203-207.doi: 10.7506/spkx1002-6630-201110048

超高效液相色谱串联质谱法同时测定水产品中6种兽药残留

隋涛，付建，李晓玉，郭海霞，娄喜山

1. 烟台出入境检验检疫局
2.烟台杰科检测服务有限公司

出版日期:2011-05-25 发布日期:2011-04-08
基金资助:
2010 年度山东检验检疫局科研项目(SK201030)

Simultaneous Determination of Veterinary Drug Residues in Aquatic Products by UPLC-MS/MS

SUI Tao1，FU Jian2，LI Xiao-yu1，GUO Hai-xia2，LOU Xi-shan2

1. Yantai Entry-exit Inspection and Quarantine Bureau, Yantai 264000, China； 2. Yantai Jieke Inspection Service Co. Ltd., Yantai 265231, China

Online:2011-05-25 Published:2011-04-08

摘要/Abstract

摘要： 采用液液萃取的前处理方式，以超高效液相色谱串联质谱(UPLC-MS/MS)检测水产品中萘啶酸、泰妙菌素、甲氧苄胺嘧啶、二氟沙星、氟甲砜霉素和吡喹酮的残留量。水产品经过匀质，乙腈提取并沉淀蛋白，正己烷去除脂肪，UPLC-MS/MS进行检测，在6min内完成分离。在5～200μg/L范围内，相关系数R2在0.9977～0.9999之间，具有良好的线性关系。6种物质的检测限度均为1.0μg/kg，回收率范围在61.2%～90.5%之间。本方法操作简单、灵敏度高，可以满足水产品中农药残留的的定性定量检测。

关键词: 吡喹酮, 超高效液相色谱串联质谱, 多反应监测, 萘啶酸, 泰妙菌素, 甲氧苄胺嘧啶, 二氟沙星, 氟甲砜霉素

Abstract: A method for detecting residues of nalidixic acid, tiamulin, trimethoprim, difloxacin, florfenicol and praziquantel in aquatic products by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)after liquid-liquid extraction approach was established. The samples were extracted using acetonitrile as the solvent, purified by hexane and detected by UPLC-MS/MS within 6 minutes. The linear regression coefficients corresponding to 6 spiked levels in the range of 5 to 200μg/L were between 0.9977 and 0.9999. The detection limit for each of the six substances was 1.0μg/kg, and their recoveries were in the range of 61.2% to 90.5%. The developed method is simple and sensitive and can meet the requirements for qualitative and quantitative analysis of aquatic products.

Key words: nalidixic acid, tiamulin, trimethoprim, difloxacin, florfenicol, praziquantel, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), multiple-reaction monitoring (MRM)

中图分类号:

隋涛，付建，李晓玉，郭海霞，娄喜山. 超高效液相色谱串联质谱法同时测定水产品中6种兽药残留[J]. 食品科学, 2011, 32(10): 203-207.

SUI Tao，FU Jian，LI Xiao-yu，GUO Hai-xia，LOU Xi-shan. Simultaneous Determination of Veterinary Drug Residues in Aquatic Products by UPLC-MS/MS[J]. FOOD SCIENCE, 2011, 32(10): 203-207.

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超高效液相色谱串联质谱法同时测定水产品中6种兽药残留

Simultaneous Determination of Veterinary Drug Residues in Aquatic Products by UPLC-MS/MS

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