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用液相色谱电化学检测法同时测定中药粉防己中的汉防己甲素和粉防己乙素。

Simultaneous determination of tetrandrine and fangchinoline in herbal medicine Stephania tetrandra S. Moore by liquid chromatography with electrochemical detection.

机构信息

Key Laboratory of Combinatorial Biosynthesis and Drug Discovery (Wuhan University), Ministry of Education, Wuhan 430071, China.

出版信息

J Pharm Biomed Anal. 2012 Mar 5;61:252-5. doi: 10.1016/j.jpba.2011.11.027. Epub 2011 Dec 6.

Abstract

A simple and selective method was developed for the simultaneous determination of tetrandrine and fangchinoline in herbal medicine by HPLC with electrochemical detection (ECD) on a bare glassy carbon electrode. The HPLC separation and ECD conditions have been optimized. The separation was carried out on a WondaSil C18-WR column (4.6 mm × 250 mm, 5 μm), with the mobile phase of acetonitrile-ammonium acetate buffer (pH 6.5; 40 mM) (32:68, v/v) using an isocratic elution at the flow rate of 0.5 mL/min. The electrochemical detection potential was set at +0.9 V. The obtained LODs for tetrandrine and fangchinoline were 0.26 and 0.27 μmol/L, respectively. The method was successfully applied to the analysis of tetrandrine and fangchinoline contents in Stephania tetrandra S. Moore. It has been demonstrated that the LC-ECD method is an excellent technique for analysis of the herbal medicine. The mean recoveries were in the range of 95-105%, while the precision expressed as repetition of peak area was lower than 2.7%.

摘要

建立了一种在裸玻碳电极上用高效液相色谱电化学检测(HPLC-ECD)同时测定中草药中粉防己碱和防己诺林碱的方法。优化了 HPLC 分离和 ECD 条件。在 WondaSil C18-WR 柱(4.6mm×250mm,5μm)上,以乙腈-乙酸铵缓冲液(pH6.5;40mM)(32:68,v/v)为流动相,流速为 0.5mL/min,采用等度洗脱进行分离。电化学检测电位设置为+0.9V。粉防己碱和防己诺林碱的检出限分别为 0.26 和 0.27μmol/L。该方法成功应用于测定粉防己和粉防己碱的含量。结果表明,LC-ECD 法是分析中草药的一种很好的技术。平均回收率在 95-105%之间,而峰面积重复的精密度低于 2.7%。

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