山东科学 ›› 2017, Vol. 30 ›› Issue (3): 17-20.doi: 10.3976/j.issn.1002-4026.2017.03.004

• 中药与天然活性产物 • 上一篇    下一篇

HPLC-MS同时测定泽泻中两种泽泻醇的含量

池雨锋1 ,王小明1 ,张玲1 ,林莎莎1 ,蒋海强2*,周洪雷1*   

  1. 1.山东中医药大学药学院,山东 济南 250355;2山东中医药大学实验中心,山东 济南 250355
  • 收稿日期:2016-08-12 出版日期:2017-06-20 发布日期:2017-06-20
  • 通信作者: 蒋海强(1982—),男,博士,副教授,研究方向为天然药物化学成分。E-mail: jhq12723@163.com; 周洪雷(1967—),男,教授,研究方向为中药及复方活性成分与质量控制。Email:zhouhongleitcm@163.com E-mail:jhq12723@163.com
  • 作者简介:池雨锋(1989—),男,硕士研究生,研究方向为天然药物化学成分。E-mail:chongming0539@126.com
  • 基金资助:

    山东省自然科学基金(ZR2015HM080);山东省博士后创新项目专项资金(201403006);山东省科技计划(2013GSF11903);山东省高校中医药抗病毒协同创新课题(XTCX2014C01-03)

Simultaneous determination of two alisols in Rhizoma Alismatis by HPLC-MS

CHI Yu-feng1,WANG Xiao-ming1,ZHANG Ling1,LIN Sha-sha1,JIANG Hai-qiang2*,ZHOU Hong-lei1*   

  1. 1.College of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250355,China;
    2.Experience Center of Shandong University of Traditional Chinese Medicine, Jinan 250355,China
  • Received:2016-08-12 Online:2017-06-20 Published:2017-06-20

摘要:

为提高泽泻药材的质量控制水平,建立了泽泻中23-乙酰泽泻醇B和24-乙酰泽泻醇A的高效液相质谱联用含量测定方法。色谱条件为Halo C18 色谱柱(2.1 mm×100 mm, 2.7 μm),体积分数0.1%甲酸水-0.1%甲酸乙腈为流动相,梯度洗脱,流速0.3 mL·min-1,柱温30 ℃;质谱条件为ESI离子源, 正离子检测方式,MRM模式,干燥气温度350 ℃,干燥气流速9 L·min-1,雾化器压力241.3 kPa,毛细管电压4 000 V。 测得药材中23-乙酰泽泻醇B和24-乙酰泽泻醇A含量分别为11.459 5 μg·g-1,321.823 9 μg·g-1。该方法结果准确,重现性好,可用于测定泽泻中两种成分的含量。

关键词: 高效液相-质谱法, 泽泻, 含量测定, 泽泻醇

Abstract:

To improve the quality control of the Rhizoma Alismatis, a HPLCMS method for  determination of the contents of two alisols in Rhizoma Alismatis was established in this paper. Chromatographic conditions were as follows:Halo C18 column(2.1 mm×100 mm, 2.7 μm), the mobile phase was a mixture of 0.1% formic acid solution0.1% formic acid in acetonitrile, gradient elution, the flow rate was 0.3 mL·min-1, the column temperature was 30 ℃. The conditions of MS included: ESI ion source, detection method with positive ions, mode by MRM, drying temperature was 350 ℃, the flow rate of drying gas was 9 L·min-1, pressure of nebulizer was 241.3 kPa, and the voltage of capillary was 4 000 V. The content of alisol B 23-acetate and alisol A 24-acetate in the samples was 11.459 5 μg·g-1 and 321.823 9 μg·g-1, respectively. The method is accurate and reproducible to the determination of two alisols in Rhizoma Alismatis.

Key words: Rhizoma Alismatis, alisols, content determination, HPLC-MS

中图分类号: 

  • R284.1