色谱

色谱 ›› 2018, Vol. 36 ›› Issue (6): 506-517.DOI: 10.3724/SP.J.1123.2018.02023

• 生物基质农兽药残留检测专栏 • 上一篇    下一篇

食品中99种兽药的一步式提取净化体系

李双1,2, 陈树兵1, 李露青1, 徐旭文1, 陈先锋1, 钟莺莺1, 张雅珩3, 王传现4   

  1. 1. 宁波出入境检验检疫局检验检疫技术中心, 浙江 宁波 315211;
    2. 宁波大学应用海洋生物技术教育部重点实验室, 浙江 宁波 315211;
    3. 甘肃出入境检验检疫局综合技术中心, 甘肃 兰州 730010;
    4. 上海出入境检验检疫局, 上海 200135
  • 收稿日期:2018-03-06 出版日期:2018-06-08 发布日期:2014-04-24
  • 通讯作者: 陈树兵,Tel:(0574)87022692,E-mail:shubingchen@126.com
  • 基金资助:

    浙江省基础公益研究计划项目（LGN18B050002）；国家质检总局科技项目（2016IK169，2016IK170，2017IK255）.

System of simultaneous extraction and cleaning of 99 veterinary drugs in food

LI Shuang1,2, CHEN Shubing1, LI Luqing1, XU Xuwen1, CHEN Xianfeng1, ZHONG Yingying1, ZHANG Yaheng3, WANG Chuanxian4   

  1. 1. Ningbo Entry-Exit Inspection and Quarantine Bureau Technology Center, Ningbo 315211, China;
    2. Key Laboratory of Applied Marine Biotechnology of Chinese Ministry of Education, Ningbo University, Ningbo 315211, China;
    3. Comprehensive Technical Center of Gansu Entry and Exit Inspection and Quarantine Bureau, Lanzhou 730010, China;
    4. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2018-03-06 Online:2018-06-08 Published:2014-04-24
  • Supported by:

    Zhejiang Provincial Basic Public Welfare Research Project (No.LGN18B050002);Science and Technology Project of General Administration of Quality Supervision,Inspection and Quarantine of the People's Republic of China (AQSIQ)(Nos.2016IK169,2016IK170,2017IK255).

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摘要：

建立了99种禁限用兽药的一步式提取净化体系，并通过高效液相色谱-四极杆/静电场轨道阱高分辨质谱（UHPLC-Q-Orbitrap HRMS）对其效果进行了评价。该提取净化体系基于载体辅助液液萃取技术，通过一次性前处理，完成常见的理化性质差异很大的8大类共计99种兽药残留的提取、净化工作，同时结合四极杆静电场轨道阱高分辨质谱实现了99种兽药残留的一步式多残留筛查。采用此体系对样品禁限用兽药进行测定分析，结果表明，该方法对液态乳、猪肉、鱼类等食品基质具有较强的适用性，检测的99种兽药线性范围为0.001~0.1 μg/mL，定量限为0.5~20.0 μg/kg，加标回收率为60%~120%，相对标准偏差小于15%。该方法的前处理和仪器分析过程对不同理化性质的化合物的兼容性强，检测效率高，可操作性强，检出限能满足所有受试的目标物，并且大大降低了检测成本。

关键词: 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱, 食品, 兽药, 载体辅助液液萃取

Abstract:

We established a system for the simultaneous extraction and cleaning of 99 veterinary drugs from food by ultra-performance liquid chromatography coupled with quadrupole electrostatic field-orbital trap-high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS). The system is based on the supported liquid-liquid extraction technology through one-off pretreatment, which covers the common eight categories of physical and chemical properties, and the extraction and purification of 99 different veterinary drug residues. At the same time, the one-step multi residue screening of 99 veterinary drug residues has been realized using HRMS. The results showed that the method was suitable for extraction from milk, pork, and fish. The 99 veterinary drugs showed a good linear relationship in the concentration range of 0.001-0.1 μg/mL, the limit of quantification was 0.5-20.0 μg/kg, the average recoveries were 60%-120%, and the relative standard deviations (RSDs) were not more than 15%. The pre-processing and instrumental analysis of this method have high detection efficiency, strong maneuver ability, and strong compatibility with different physical and chemical compounds. Moreover, the detection limit can meet all the objects of the test and greatly reduce the detection cost.

Key words: carrier supported liquid-liquid extraction, food, ultra performance liquid chromatography coupled with quadrupole electrostatic field-orbital trap-high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS), veterinary drugs

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