色谱

色谱 ›› 2012, Vol. 30 ›› Issue (11): 1153-1158.DOI: 10.3724/SP.J.1123.2012.06040

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱同时测定加味左金丸中的9种有效成分

覃莎1,2, 王锦2, 徐远金1,2*   

  1. 1. 亚热带农业生物资源保护与利用国家重点实验室, 广西大学, 广西 南宁 530004; 2. 广西大学化学化工学院, 广西 南宁 530004
  • 收稿日期:2012-06-28 修回日期:2012-08-07 出版日期:2012-11-28 发布日期:2012-11-21
  • 通讯作者: 徐远金,博士,教授,研究方向为色谱、质谱分析. Tel: (0771)3237743, E-mail: yjxu@gxu.edu.cn.
  • 基金资助:

    广西自然科学基金项目(桂科自0832034).

Simultaneous determination of nine effective components in Jiaweizuojin Pills by ultra performance liquid chromatography with tandem mass spectrometry

QIN Sha1,2, WANG Jin2, XU Yuanjin1,2*   

  1. 1. State Key Laboratory of Conservation and Utilization of Subtropical Agro-bioresources, Guangxi University, Nanning 530004, China; 2. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China
  • Received:2012-06-28 Revised:2012-08-07 Online:2012-11-28 Published:2012-11-21

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424

被引次数

23

摘要： 建立了同时测定加味左金丸中9种药效成分含量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。采用Zorbax RRHD Eclipse Plus C18色谱柱,以含0.2%甲酸的水-甲醇为流动相进行梯度洗脱,流速0.4 mL/min,在电喷雾电离(ESI)正离子模式下,采用多重反应监测模式进行检测。结果表明,芍药苷、延胡索乙素、药根碱、小檗碱、巴马汀、吴茱萸碱、柴胡皂苷C、柴胡皂苷A、柴胡皂苷D的线性范围分别为0.025～5.0 mg/L、0.0010～2.0 mg/L、0.0023～7.2 mg/L、0.0027～28.9 mg/L、0.0023～9.1 mg/L、0.0050～1.0 mg/L、0.050～10 mg/L、0.005～1.0 mg/L、0.0075～1.5 mg/L;检出限分别为5.0、0.20、0.45、0.54、0.45、1.0、10、1.0、1.5 μg/L。9种成分的加样回收率为99.3%～105%,相对标准偏差均不大于2.6%。该法快捷、准确、重复性好,已成功用于实际样品的分析。

关键词: 超高效液相色谱-串联质谱(UPLC-MS/MS), 加味左金丸, 有效成分, 中成药

Abstract: A method for the simultaneous determination of paeoniflorin, tetrahydropalmatine, jatrorrhizine, berberine, palmatine, evodiamine, saikosaponin C, saikosaponin A and saikosaponin D in Jiaweizuojin Pills was established by ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS). The UPLC separation was performed on a Zorbax RRHD Eclipse Plus C18 column (50 mm×2.1 mm, 1.8 μm) by using 0.2% (v/v) formic acid aqueous solution and methanol as mobile phases with the gradient elution at a flow rate of 0.4 mL/min. The analytes were detected by tandem mass spectrometry under the positive ion mode with the electrospray ionization (ESI) source and in the multiple reaction monitoring (MRM) mode. Under the optimized conditions, the calibration curves were linear in the ranges of 0.025~5.0 mg/L for paeoniflorin, 0.0010~2.0 mg/L for tetrahydropalmatine, 0.0023~7.2 mg/L for jatrorrhizine, 0.0027~28.9 mg/L for berberine, 0.0023~9.1 mg/L for palmatine, 0.0050~1.0 mg/L for evodiamine, 0.050~10 mg/L for saikosaponin C, 0.0050~1.0 mg/L for saikosaponin A and 0.0075~1.5 mg/L for saikosaponin D with the detection limits of 5.0, 0.20, 0.45, 0.54, 0.45, 1.0, 10, 1.0, 1.5 μg/L, respectively. The average recoveries of the nine effective components were between 99.3% and 105% with the relative standard deviations not more than 2.6%. The developed method is simple, rapid and accurate, and suitable for the quality control of the nine effective components in Jiaweizuojin Pills.

Key words: Chinese patent drug, effective components, Jiaweizuojin Pills, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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