色谱

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亲水作用色谱法测定胡芦巴中的胡芦巴碱

卓荣杰1, 王莉1, 王龙星1, 肖红斌1*, 蔡少青2   

  1. 1. 中国科学院大连化学物理研究所, 辽宁 大连 116023; 2. 北京大学药学院, 北京 100083
  • 收稿日期:2009-11-23 修回日期:2010-01-22 出版日期:2010-04-28 发布日期:1980-12-25
  • 通讯作者: 肖红斌

Determination of trigonelline in Trigonella foenum-graecum L. by hydrophilic interaction chromatography

ZHUO Rongjie1, WANG Li1, WANG Longxing1, XIAO Hongbin1*, CAI Shaoqing2   

  1. 1. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;2. School of Pharmaceutical Sciences of Peking University, Beijing 100083, China
  • Received:2009-11-23 Revised:2010-01-22 Online:2010-04-28 Published:1980-12-25
  • Contact: XIAO Hongbin

摘要: 建立了亲水作用色谱法(HILIC)测定胡芦巴药材中胡芦巴碱含量的方法。采用Waters Atlantis HILIC Silica色谱柱(150 mm×2.1 mm, 3 μm),以乙腈-乙酸铵溶液(pH 4.4)(体积比为70:30)为流动相,流速0.4 mL/min,检测波长265 nm。胡芦巴碱的线性范围为2.50~100 mg/L (r=0.9996);两个加标水平的平均加样回收率为102%,相对标准偏差(RSD)分别为4.17%和2.28%(n=3)。结果表明所建方法分离效果好、快速简易,可以弥补中国药典中离子对色谱法(IPLC)平衡时间过长的缺陷,适用于胡芦巴药材中强极性胡芦巴碱的测定,为胡芦巴的质量控制提供了有效的方法。

关键词: 胡芦巴, 胡芦巴碱, 亲水作用色谱法, 中药材

Abstract: A method of hydrophilic interaction chromatography (HILIC) was established for the quantitative determination of trigonelline in Trigonella foenum-graecum L. HILIC analysis was performed on a Waters Atlantis HILIC Silica column (150 mm×2.1 mm, 3 μm). The mobile phase consisted of acetonitrile-ammonium acetate (pH 4.4) (70:30, v/v), and the flow rate was 0.4 mL/min. The detection wavelength was set at 265 nm. The method has good linearity in the range of 2.50~100 mg/L for trigonelline (r=0.9996). The recoveries were on an average of 102%by adding 29.2 mg/L and 43.8 mg/L with relative standard deviations (RSDs) of 4.17% and 2.28% (n=3), respectively. The results indicate that the method is simple and rapid for the determination of strong polar trigonelline in Trigonella foenum-graecum L. Furthermore, it significantly reduces the equilibration time compared with ion-pair liquid chromatography (IPLC) recorded in the Pharmacopoeia of China. This new method can be used as a valid method for the quality control of Trigonella foenum-graecum L.

Key words: traditional Chinese medicine (TCM) , Trigonella foenum-graecum L., trigonelline, hydrophilic interaction chromatography (HILIC)