色谱

色谱 ›› 2014, Vol. 32 ›› Issue (3): 216-223.DOI: 10.3724/SP.J.1123.2013.11008

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱双内标法同时测定复方杏香兔耳风胶囊中的10种有效成分

范晓苏1,2, 庞倩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:2013-11-04 修回日期:2013-12-16 出版日期:2014-03-08 发布日期:2014-03-04
  • 通讯作者: 徐远金
  • 基金资助:

    广西自然科学基金项目（桂科自0832034）.

Simultaneous determination of ten constituents in the Chinese medicinal preparation Fufangxingxiangtu’erfeng capsules by ultra performance liquid chromatography with tandem mass spectrometry

FAN Xiaosu1,2, PANG Qian2, 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:2013-11-04 Revised:2013-12-16 Online:2014-03-08 Published:2014-03-04

PDF

341

被引次数

7

摘要：

建立了同时测定复方杏香兔耳风胶囊中原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸C、黄芩苷、木犀草素、芹菜素、白术内酯Ⅲ和白术内酯I等10种有效成分含量的超高效液相色谱-串联质谱（UPLC-MS/MS）双内标分析方法。以咖啡酸和淫羊藿苷为内标（IS），在ZORBAX RRHD Eclipse Plus C18色谱柱上，以甲醇和含0.3%甲酸的水为流动相进行梯度洗脱分离，流速为0.3 mL/min。在电喷雾电离（ESI）正、负离子切换模式下，采用多重反应监测模式进行检测。结果表明，原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸C、黄芩苷、木犀草素、芹菜素、白术内酯Ⅲ、白术内酯I的线性范围分别为0.00300~24.0 mg/L、0.0170~2.00 mg/L、0.0150~30.0 mg/L、0.00400~30.0 mg/L、0.0105~24.0 mg/L、0.00300~30.0 mg/L、0.00300~5.00 mg/L、0.00600~5.00 mg/L、0.00150~4.00 mg/L、0.000600~0.900 mg/L；检出限分别为1.0、11、5.0、1.5、3.5、1.0、1.0、2.0、0.50、0.20 μg/L。10种成分的加样回收率为92.5%~106%，相对标准偏差均不大于3.2%。该方法快速简便、灵敏度高、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, 复方杏香兔耳风胶囊, 有效成分

Abstract:

Using caffeic acid and icariin as internal standards, a method for the simultaneous determination of protocatechuic acid, protocatechuic aldehyde, chlorogenic acid, scutellarin, isochlorogenic acid C, baicalin, luteolin, apigenin, atractylenolide Ⅲ and atractylenolide I in Fufangxingxiangtu'erfeng capsules were established by ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS). The separation was performed on a ZORBAX RRHD Eclipse Plus C18 column (50 mm×2.1 mm, 1.8 μm) by using water containing 0.3% formic acid and methanol as mobile phases with the gradient elution at a flow rate of 0.3 mL/min. The analytes were detected by a tandem mass spectrometer in the multiple reaction monitoring (MRM) mode via the switching of positive electrospray ionization (ESI+) and negative electrospray ionization (ESI-). Under optimum conditions, the calibration curves were linear in the range of 0.00300-24.0 mg/L for protocatechuic acid, 0.0170-2.00 mg/L for protocatechuic aldehyde, 0.0150-30.0 mg/L for chlorogenic acid, 0.00400-30.0 mg/L for scutellarin, 0.0105-24.0 mg/L for isochlorogenic acid C, 0.00300-30.0 mg/L for baicalin, 0.00300-5.0 mg/L for luteolin, 0.00600-1.50 mg/L for apigenin, 0.00150-4.00 mg/L for atractylenolide Ⅲ, and 0.000600-0.900 mg/L for atractylenolide I with the detection limits of 1.0, 11, 5.0, 1.5, 3.5, 1.0, 1.0, 2.0, 0.50, 0.20 μg/L, respectively. The average recoveries of the ten effective components were between 92.5% and 106% with all relative standard deviations not more than 3.2%. The developed method was rapid, simple, accurate, reproducible, and suitable for the quality control of the Fufangxingxiangtu'erfeng capsules.

Key words: effective components, Fufangxingxiangtu’erfeng capsules, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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