色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 46-53.DOI: 10.3724/SP.J.1123.2018.08046

• 特别策划：南京海关动植物与食品检测中心专栏 • 上一篇    下一篇

液相色谱-串联质谱法检测雄蜂蛹粉中50种抗生素残留

杨雯筌1, 张晓燕1, 姚倩1, 周杨娟2, 胡亚文2, 王茂华3, 唐茂芝3   

  1. 1. 南京海关动植物与食品检测中心, 江苏 南京 210001;
    2. 东南大学成贤学院, 江苏 南京 210088;
    3. 国家认证认可监督管理委员会认证认可技术研究所, 北京 100020
  • 收稿日期:2018-09-10 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 张晓燕,Tel:(025)52345187,E-mail:zhangxiaoyan8196@126.com.
  • 基金资助:

    国家重点研发计划课题（2018YFF0215605）.

Determination of 50 antibiotic residues in drone pupa powder by liquid chromatography-tandem mass spectrometry

YANG Wenquan1, ZHANG Xiaoyan1, YAO Qian1, ZHOU Yangjuan2, HU Yawen2, WANG Maohua3, TANG Maozhi3   

  1. 1. Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210001, China;
    2. Southeast University Chengxian College, Nanjing 210088, China;
    3. China Certification & Accreditation Institute, Beijing 100020, China
  • Received:2018-09-10 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    National Key Research and Development Program (No. 2018YFF0215605).

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摘要：

建立了液相色谱-串联质谱检测雄蜂蛹粉中50种抗生素残留（大环内酯类、喹诺酮类、磺胺类、四环素类、硝基咪唑类、林可霉素和氯霉素）的方法。样品经高氯酸溶液和醋酸铅溶液提取沉淀蛋白质，清液用磷酸氢二钾溶液调节pH值至8，经固相萃取净化后进行仪器分析。采用多反应监测正离子或负离子模式检测，可以一次完成对雄蜂蛹粉中50种目标化合物的定性和定量测定。50种抗生素的加标回收率为70.2%~118.3%，相对标准偏差（RSD）为1.8%~13.6%。该方法操作简便，灵敏度高，适用于雄蜂蛹粉中多种兽药残留的分析确证。

关键词: 固相萃取, 抗生素残留, 雄蜂蛹粉, 液相色谱-串联质谱

Abstract:

A method was established for the determination of 50 kinds of antibiotic residues (macrolides, quinolones, sulfonamides, tetracyclines, nitroimidazoles, lincomycin and chloramphenicol) in drone pupa powder by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with perchloric acid and lead acetate solution, and the protein was precipitated. The extraction solution was adjusted to pH 8 using dipotassium hydrogen phosphate, then the solution was purified by solid phase extraction (SPE) and analyzed by LC-MS/MS. The target compounds in the drone pupa powder were determined quantitatively and quantitatively by using multiple reaction monitoring and positive ion or negative ion modes. The recoveries of the 50 antibiotics were in the range of 70.2%-118.3%, and the relative standard deviations (RSDs) were 1.8%-13.6%. The method is simple, selective, and can be suitable for the analysis and confirmation of veterinary drug residues in drone pupa powder.

Key words: antibiotic residues, drone pupa powder, liquid chromatography-tandem mass spectrometry (LC-MS/MS), solid phase extraction (SPE)

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