色谱

色谱

• 研究论文 • 上一篇    下一篇

反相高效液相色谱法测定康肾颗粒中的葛根素

陈曼1,史键2,王骊丽1,耿信笃1   

  1. 1.Shaanxi Key Laboratory of Modern Separation Science, Institute of Modern Separation Science, Northwest University, Xi’an 710069, China; 2.Department of Nephropathy, Shaannxi Academy of Traditional Chinese Medicine,  Xi’an 710003, China
  • 收稿日期:2005-11-25 修回日期:2006-02-21 出版日期:2006-09-30 发布日期:1986-09-25
  • 通讯作者: 耿信笃

Determination of Puerarin in Kangshen Granule by Reversed-Phase High Performance Liquid Chromatography

CHEN Man1, SHI Jian2, WANG Lili1, GENG Xindu1   

  1. 1.Shaanxi Key Laboratory of Modern Separation Science, Institute of Modern Separation Science, Northwest University, Xi’an 710069, China; 2.Department of Nephropathy, Shaannxi Academy of Traditional Chinese Medicine,  Xi’an 710003, China
  • Received:2005-11-25 Revised:2006-02-21 Online:2006-09-30 Published:1986-09-25
  • Contact: GENG Xindu

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680

被引次数

39

摘要： 建立了反相高效液相色谱分离、质谱定性、紫外检测定量测定康肾颗粒中葛根素含量的方法。采用YMC-ODS色谱柱(4.6 mm i.d.×100 mm,10 μm),选用甲醇(含0.1%三氟醋酸)和水(含0.1%三氟醋酸)体系为流动相,非线性梯度洗脱分离,流速1.0 mL/min,检测波长250 nm；用基质辅助激光解吸离子化飞行时间质谱(MALDI-TOF MS)分析鉴定对照品和样品的馏分,在确定目标峰后进行紫外检测定量测定。结果表明，葛根素在0.132 ~1.32 μg范围内其峰面积与进样量呈良好的线性关系（r=0.9997）,平均加标回收率高于103%,相对标准偏差低于2.0%(n=6)。应用该方法测定康肾颗粒中葛根素，其平均含量为3.09 mg/g。该方法简单、快速、重现性好。

关键词: 反相高效液相色谱法, 葛根素, 基质辅助激光解吸离子化飞行时间质谱, 康肾颗粒 , 紫外检测

Abstract: Kangshen granule, containing 12 kinds of traditional Chinese medicine, has complex composition. A new method for the determination of puerarin in Kangshen granule was developed using reversed-phase high performance liquid chromatography coupled with matrix assisted laser desorption ionization time of flight mass spectrometry and ultraviolet detection (RP-HPLC/MALDI-TOF MS/UV). The sample was separated by RP-HPLC with a non-linear gradient elution, and then was qualitatively detected by mass spectrometry to identify the puerarin peak. The chromatographic process was performed on a YMC-ODS column under the optimized conditions with a mobile phase consisting of methanol, water and 0.1% TFA, and detected at 250 nm. The linear range of puerarin was from 0.132 to 1.32 μg (r=0.9997). The recovery was higher than 103% and the relative standard deviation was lower than 2.0% (n=6). The puerarin content in Kangshen granule sample was determined and the puerarin content was 3.09 mg/g. The method is simple and feasible for the determination of puerarin with a good repeatability. The method can be used for quality control of Kangshen granule.

Key words: Kangshen granule , matrix assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS), puerarin, ultraviolet detection, reversed-phase high performance liquid chromatography (RP-HPLC)