色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 898-902.DOI: 10.3724/SP.J.1123.2013.02028

• 技术与应用 • 上一篇    下一篇

固相萃取-超高效液相色谱-电喷雾串联质谱法同时检测尿样中的麻黄碱和N-甲基麻黄碱

张琳1, 张福成2, 王朝虹3, 蒋晔1, 许萌1, 李虹4   

  1. 1. 河北医科大学药学院, 河北 石家庄 050017;
    2. 空军总医院, 北京 100142;
    3. 最高人民检察院司法鉴定中心, 北京 100040;
    4. 云南省公安厅刑警总队, 云南 昆明 650000
  • 收稿日期:2013-02-25 修回日期:2013-04-14 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 蒋晔
  • 基金资助:

    河北省卫生厅科研基金项目(08056).

Simultaneous determination of ephedrine and N-methylephedrine in urine by solid phase extraction-ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

ZHANG Lin1, ZHANG Fucheng2, WANG Zhaohong3, JIANG Ye1, XU Meng1, LI Hong4   

  1. 1. School of Pharmacology, Hebei Medical University, Shijiazhuang 050017, China;
    2. Air Force General Hospital, Beijing 100142, China;
    3. Institute of Forensic Science of Supreme People's Procuratorate, Beijing 100040, China;
    4. Interpol Corps of Yunnan Public Security Bureau, Kunming 650000, China
  • Received:2013-02-25 Revised:2013-04-14 Online:2013-09-28 Published:2013-09-02

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摘要：

建立了固相萃取-超高效液相色谱-电喷雾串联质谱(SPE-UPLC-ESI MS/MS)联用方法,定量测定尿样中的麻黄碱和N-甲基麻黄碱。样品经Oasis MCX柱提取、纯化和富集后,采用电喷雾(ESI)离子源电离,正离子多反应监测(MRM)模式质谱进行定性和定量分析。麻黄碱和N-甲基麻黄碱在0.0250~2.50 μg/L质量浓度范围内线性关系良好,线性相关系数分别为0.9998和0.9992,提取回收率高于80%,提取效率的RSD小于5.0%,检出限均达到0.01 μg/L,可大大延长尿样检材中麻黄碱和N-甲基麻黄碱的检测周期。结果表明,该方法快速、准确,为尿液中痕量麻黄碱和N-甲基麻黄碱的分析提供了灵敏的分析方法。

关键词: N-甲基麻黄碱, 超高效液相色谱-电喷雾串联质谱, 固相萃取, 麻黄碱, 尿

Abstract:

A rapid and sensitive method has been developed for the simultaneous determination of ephedrine and N-methylephedrine in urine samples by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-ESI MS/MS). The samples were extracted with Oasis MCX solid phase extraction cartridges and measured in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). Good linearities were observed in the range of 0.0250-2.50 μg/L with correlation coefficient over 0.9990 for both analytes. The recoveries were above 80% with RSDs less than 5.0%. The limits of detection were 0.01 μg/L. The method proves to be rapid and sensitive for the trace determination of ephedrine and N-methylephedrine in urine samples.

Key words: N-methylephedrine, ephedrine, solid phase extraction (SPE), ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI MS/MS), urine

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