HPLC法测定常山口服溶液的主成分含量

Determination of the Main Components for Dichroae Radix(CHANG SHAN) Oral Liquid by HPLC Method

为建立一种同时测定常山口服液中2种主成分的高效液相色谱方法(HPLC),对中药常山及其药物制剂的国家兽药典质量标准提出制修订建议。本研究采用HPLC法,通过方法学验证和不同色谱检测系统的考察,测定常山口服液中常山乙素和常山甲素的含量,明确药物色谱条件的系统适用性要求。包括安捷伦1290型HPLC仪(SB-C_(18)色谱柱)、沃特斯2695型HPLC仪(XTerra@MS C_(18)色谱柱)和岛津SPD-10A型HPLC仪(Amethyst C_(18)-H色谱柱);流动相:乙腈-水-冰醋酸(30∶69.79∶0.21),pH值5.2~6.2,流速:1.0 mL/min,检测波长:265 nm,柱温:25℃,进样量:10μL。三种不同类型的液相系统和色谱柱,所测3批次样品中的主成分含量基本一致,常山甲素和常山乙素的峰型较好,与周围杂质可有效分离。该研究方法可为常山碱口服液质量控制提供参考。

The purpose of the present study was to develop a high performance liquid chromatography (HPLC) method for the simultaneous determination of two main components in Chang Shan Oral Liquid (CSOL),and to make recommendations for the revision of the National Veterinary Pharmacopoeia's quality standards about Dichroae radix and its pharmaceutical preparations.Three different types of liquid phase and chromatographic column were chosen in this study including Agilent 1290 type liquid chromatography (SB-C_(18) chromatographic column),Waters 2695 type liquid chromatography (XTerra@MS C_(18) chromatographic column),and Island ferry SPD-10A type liquid chromatography (Amethyst C_(18)-H chromatographic column).Mobile phase consisted of acetonitrile-H_2O-glacial acetic acid (30:69.79:0.21) at pH5.2~6.2 (adjusted with triethylamine) and velocity of 1.0 mL/min.The operational conditions included the detection wavelength at 265 nm,column temperature at 25℃and injection volume of 10μL.The results showed that the contents of the main components in three batches of CSOL were similar and better peak type and separation effect were obtained from three types of HPLC and chromatographic column conditions.This HPLC method was simple,rapid,sensitive and specific to be used for the determination on the contents of β-dichroine and α-dichroine in Dichroae radix in CSOL.