色谱

色谱 ›› 2018, Vol. 36 ›› Issue (2): 114-124.DOI: 10.3724/SP.J.1123.2017.10010

• 研究论文 • 上一篇    下一篇

QuEChERS-超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速测定水产品中25种药物残留

张宪臣1, 李蓉1, 张朋杰1, 吴霞2, 华洪波3, 杨璐齐1, 卢俊文1, 容裕棠1   

  1. 1. 中山出入境检验检疫局检验检疫技术中心, 广东 中山 528403;
    2. 安捷伦科技(中国)有限公司, 广东 广州 510000;
    3. 中山市卓雅外语学校, 广东 中山 528401
  • 收稿日期:2017-10-12 出版日期:2018-02-08 发布日期:2014-01-17
  • 通讯作者: 张宪臣,Tel:(0760)88887380,E-mail:zhangxc@zs.gdciq.gov.cn
  • 基金资助:

    广东省科技计划项目（2015A050502010）；国家质检总局科技计划项目（2015IK052）；中山市社会公益重大项目（2017B1029）；广东检验检疫局科技计划项目（2017GDK24）.

Rapid determination of 25 drug residues in aquatic products by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

ZHANG Xianchen1, LI Rong1, ZHANG Pengjie1, WU Xia2, HUA Hongbo3, YANG Luqi1, LU Junwen1, RONG Yutang1   

  1. 1. Inspection and Quarantine Technology Center of Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528403, China;
    2. Agilent Technologies Co., Ltd. (China), Guangzhou 510000, China;
    3. Zhongshan ZhuoYa Foreign Language School, Zhongshan 528401, China
  • Received:2017-10-12 Online:2018-02-08 Published:2014-01-17
  • Supported by:

    Science and Technology Plan Project of Guangdong Province of China (No.2015A050502010);Science and Technology Plan Project of General Administration of Quality Supervision Inspection and Quarantine (AQSIQ) of China (No.2015IK052);Social Public Welfare Project of Zhongshan City (No.2017B1029);Science and Technology Plan Project of Entry-Exit Inspection and Quarantine (CIQ) of Guangdong (No.2017GDK24).

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摘要：

采用了一种高效基质脂肪吸附剂（EMR-Lipid）去除水产品基质中的脂肪和磷脂等杂质，利用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法（UPLC-Q Orbitrap HRMS）的同时定性定量功能，建立了水产品中25种药物残留的检测方法。样品经乙腈提取，EMR-Lipid净化，同时加入3 g氯化钠和3 g无水硫酸钠进行盐析，采用ACQUITY UPLC BEH C18色谱柱（100 mm×2.1 mm，1.7 μm）分离，以含0.1%（v/v）甲酸的乙腈溶液和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，在加热电喷雾离子（HESI）源、全扫描/实时二级质谱扫描（Full MS/dd-MS2）监测模式下进行检测。结果表明，25种目标化合物的质量浓度与母离子峰面积间的线性关系良好，相关系数（r）均大于0.997；25种目标化合物的检出限为0.1~1.0 μg/kg，其平均加标回收率为70.1%~108.9%，相对标准偏差为2.1%~13.8%。该法具有操作简单快捷、灵敏度高等优点。

关键词: QuEChERS, 超高效液相色谱, 高效基质脂肪吸附剂, 水产品, 四极杆/静电场轨道阱高分辨质谱, 药物残留

Abstract:

An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q Orbitrap HRMS) method was developed for the rapid screening of 25 drug residues in aquatic products by the application of a novel enhanced matrix removal of lipids (EMR-Lipid). The samples were extracted with acetonitrile, cleaned-up with EMR-Lipid, and salted out with 3.0 g sodium chloride and 3.0 g sodium sulfate. The separation of the 25 drug residues was performed on an ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) with gradient elution. Acetonitrile containing 0.1% (v/v) formic acid and 0.1% (v/v) formic acid aqueous solution were used as mobile phases. The compounds were detected by Full scan/date dependent MS/MS (Full MS/dd-MS2) via heated electrospray ionization (HESI) source. The calibration curves were linear with correlation coefficients (r) greater than 0.997. The limits of detection (LODs) ranged from 0.1 μg/kg to 1.0 μg/kg. The average spiked recoveries of the 25 target compounds were between 70.1% and 108.9% with relative standard derivations (RSDs) from 2.1% to 13.8%. Compared with the previous methods, this method has characteristics of simpler sample preparation and higher sensitivity.

Key words: aquatic products, drug residues, enhanced matrix removal of lipids (EMR-Lipid), quadrupole/electrostatic field orbitrap high resolution mass spectrometry (Q Orbitrap HRMS), QuEChERS, ultra performance liquid chromatography (UPLC)

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