色谱

色谱 ›› 2014, Vol. 32 ›› Issue (8): 822-826.DOI: 10.3724/SP.J.1123.2014.03032

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定中成药和保健品中9种抗抑郁药物

勾新磊1, 高峡1,2, 胡光辉1, 刘伟丽1,2   

  1. 1. 北京市理化分析测试中心, 北京 100089;
    2. 国家食品质量安全监督检验中心, 北京 100094
  • 收稿日期:2014-03-21 修回日期:2014-04-04 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 高峡，E-mail：gaoxia@iccas.ac.cn
  • 基金资助:

    北京市自然科学基金项目（2122018）；北京市科学技术研究院创新团队计划项目（IG200801N/C2）.

Simultaneous determination of nine antidepressants in traditional Chinese medicines and health food by ultra performance liquid chromatography with tandem mass spectrometry

GOU Xinlei1, GAO Xia1,2, HU Guanghui1, LIU Weili1,2   

  1. 1. Beijing Centre for Physical and Chemical Analysis, Beijing 100089, China;
    2. China Food Quality Safety Supervision and Inspection Center, Beijing 100094, China
  • Received:2014-03-21 Revised:2014-04-04 Online:2014-08-08 Published:2014-08-01

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摘要：

建立了同时测定中成药和保健品中9种抗抑郁药物的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。以甲醇为提取溶剂，超声提取，离心后取上清液，使用Waters ACQUITY UPLC BEH C18色谱柱（100 mm×2.1 mm，1.7 μm）进行分离，以乙腈和0.1%（v/v）甲酸水为流动相对目标物进行梯度洗脱。在电喷雾正离子模式下，采用多反应监测（MRM）模式进行定性和定量分析。结果表明，9种抗抑郁药物在0.04~20 μg/L范围内线性关系良好，线性相关系数（R2）均大于0.998；目标物的检出限为0.0068~0.034 μg/L；在0.5、1、5 μg/L 3个添加水平下的平均回收率为77.7%~100.8%，相对标准偏差为0.9%~9.1%。本方法准确、简便、快速，可用于中成药和保健品中抗抑郁药物的检测。

关键词: 保健品, 超高效液相色谱-串联质谱, 抗抑郁药物, 中成药

Abstract:

A sensitive method was developed for the simultaneous determination of nine antidepressants in traditional Chinese medicines and health food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) based on the sonication-assisted extraction. The separation was performed on a Waters ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) by using 0.1% (v/v) formic acid aqueous solution and acetonitrile as the mobile phases with gradient elution at a flow rate of 0.2 mL/min. The electrospray ionization (ESI) source in positive ion mode was used for the analysis of the nine antidepressants in the multiple reaction monitoring (MRM) mode. The standard curves for the nine antidepressants were obtained with good correlation coefficients (R2>0.998) in the concentration range of 0.04-20 μg/L. The limits of detection for the nine antidepressants were in the range of 0.0068-0.034 μg/L. The average recoveries at three spiked levels (0.5, 1, 5 μg/L) were 77.7%-100.8% with the relative standard deviation of 0.9%-9.1%. The method is accurate, simple, rapid and feasible for the simultaneous determination of the antidepressants in traditional Chinese medicines and health food.

Key words: antidepressants, health food, traditional Chinese medicines, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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