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采用反相高效液相色谱-脉冲安培检测法分析柴胡及柴胡疏肝散中的柴胡皂苷。

Analysis of saikosaponins in Bupleuri Radix and Caihu-shugan-san using reversed-phase HPLC with pulsed amperometric detection.

机构信息

Department of Preventive and Social Dentistry, Graduate School, Kyung Hee University, Seoul, South Korea.

出版信息

J Sep Sci. 2011 Mar;34(6):651-8. doi: 10.1002/jssc.201000784. Epub 2011 Feb 11.

DOI:10.1002/jssc.201000784
PMID:21312331
Abstract

A simple and sensitive reversed-phase (RP) HPLC coupled with pulsed amperometric detection (PAD) method was developed to determine the saikosaponin content in Bupleuri Radix or Caihu-shugan-san. Four saikosaponins in Bupleuri Radix and Caihu-shugan-san were extracted with a 6:4 solution of 10 mM sodium phosphate buffer (pH 8)/100% ethanol. Pulsed amperometric detection of carbohydrates in four major saikosaponins was highly sensitive when used with a water-acetonitrile gradient on an alkaline RP column with a post-column delivery system. The limits of detection (S/N=3) and of quantification (S/N=10) of saikosaponins were 0.01-0.02 and 0.03-0.05 μg/mL, respectively. The intra- and inter-day precision (RSDs) were each <9.7% and the average recoveries were 95.0-97.6% in Bupleuri Radix. This method can be used to analyze saikosaponins in Bupleuri Radix and Caihu-shugan-san.

摘要

建立了一种简单灵敏的反相高效液相色谱法(RP-HPLC)结合脉冲安培检测(PAD)方法,用于测定柴胡或柴胡疏肝散中柴胡皂苷的含量。采用 6:4 的 10 mM 磷酸钠缓冲液(pH 8)/100%乙醇溶液从柴胡和柴胡疏肝散中提取 4 种柴胡皂苷。在碱性 RP 柱上采用水-乙腈梯度洗脱和柱后输送系统,对 4 种主要柴胡皂苷中的碳水化合物进行脉冲安培检测,具有很高的灵敏度。柴胡皂苷的检测限(S/N=3)和定量限(S/N=10)分别为 0.01-0.02 和 0.03-0.05 μg/mL。在柴胡中,日内和日间精密度(RSD)均<9.7%,平均回收率为 95.0-97.6%。该方法可用于分析柴胡和柴胡疏肝散中的柴胡皂苷。

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