色谱

色谱 ›› 2014, Vol. 32 ›› Issue (7): 702-706.DOI: 10.3724/SP.J.1123.2014.03002

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法同时测定猪肉中20种精神药物残留

孙婷1, 王鹭骁1, 曾三妹1, 吴敏1, 严丽娟1, 张峰2, 黄志强3   

  1. 1. 厦门出入境检验检疫局, 福建 厦门 361012;
    2. 中国检验检疫科学研究院, 北京 100025;
    3. 湖南出入境检验检疫局, 湖南 长沙 410004
  • 收稿日期:2014-03-04 修回日期:2014-04-15 出版日期:2014-07-08 发布日期:2014-06-25
  • 通讯作者: 严丽娟，E-mail：yanlj@xmciq.gov.cn；Tel:(0751)85627801；黄志强，E-mail：huangzq@hnciq.gov.cn.
  • 基金资助:

    国家科技支撑计划项目（2009BADB9B02，2012BAK08B01）；国家重大科学仪器设备开发专项项目（2012YQ14000806）.

Simultaneous determination of twenty psychoactive drugs in pork by solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

SUN Ting1, WANG Luxiao1, ZENG Sanmei1, WU Min1, YAN Lijuan1, ZHANG Feng2, HUANG Zhiqiang3   

  1. 1. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China;
    2. Chinese Academy of Inspection and Quarantine, Beijing 100025, China;
    3. Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha 410004, China
  • Received:2014-03-04 Revised:2014-04-15 Online:2014-07-08 Published:2014-06-25

PDF

429

被引次数

8

摘要：

建立了固相萃取和超高效液相色谱-电喷雾串联质谱（UPLC-ESI-MS/MS）同时测定猪肉中20种精神药物残留的方法。样品采用碱性乙腈作为提取试剂，提取液经Oasis MCX固相萃取柱净化后，以含0.1%（v/v）甲酸的水溶液和乙腈作为流动相梯度洗脱，用C18色谱柱分离，正离子模式扫描，多反应监测模式检测。20种化合物在5~100 μg/L质量浓度范围内均呈良好的线性关系，线性相关系数均大于0.99，以S/N≥10计算方法的定量限为5 μg/kg。在空白猪肉中添加5、10和50 μg/kg水平的20种药物，其平均回收率为66.8%~97.2%，相对标准偏差（RSD）为4.2%~12.4%。本方法快速、准确、可靠，适用于猪肉中精神药物多残留的同时测定。

关键词: 超高效液相色谱-电喷雾串联质谱, 固相萃取, 精神药物, 猪肉

Abstract:

A method for the simultaneous determination of 20 psychoactive drugs in pork by solid phase extraction coupled with ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was established. The samples were extracted with alkalified acetonitrile, and then cleaned up using solid phase extraction with an Oasis MCX column. The UPLC separation was performed on a C18 column (50 mm×2.1 mm, 1.7 μm) using a gradient elution with the mobile phases of 0.1% (v/v) formic acid in water and acetonitrile. The ESI-MS/MS detection was achieved in positive mode under multiple reaction monitoring (MRM) mode. The calibration curves showed good linearity in the range of 5-100 μg/L with the correlation coefficients more than 0.99 for the 20 psychoactive drugs. The limits of quantification (LOQ, S/N≥10) for the 20 psychoactive drugs were 5 μg/kg. The average recoveries of the 20 psychoactive drugs spiked in blank pork at three levels of 5, 10 and 50 μg/kg were 66.8%-97.2% with the relative standard deviations from 4.2% to 12.4%. The method is suitable for the simultaneous determination of the 20 psychoactive drugs in pork with the characteristics of easy operation, high accuracy and precision.

Key words: pork, psychoactive drugs, solid phase extraction (SPE), ultra performance liquid chromatography-electrospary ionization tandem mass spectrometry (UPLC-ESI-MS/MS)

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