川菊止痛胶囊的质量标准研究

Study on Quality Standard for Chuanju Zhitong Capsule

目的建立川菊止痛胶囊质量标准。方法采用薄层色谱法对复方中柴胡、菊花进行定性鉴别。HPLC同时测定制剂中黄芩苷、黄芩素、汉黄芩苷、汉黄芩素及甘草苷含量,色谱柱:Kromasil 100-5C_(18)(250 mm×4.6 mm,5μm);流动相:乙腈-0.05%磷酸溶液,梯度洗脱;检测波长为280 nm;流速:1.0 mL·min^(-1);进样量:10μL。结果薄层色谱斑点清晰且阴性样品无干扰。甘草苷、黄芩苷、黄芩素、汉黄芩苷及汉黄芩素分别在10.7～107μg·mL^(-1)、12.12～121.2μg·mL^(-1)、11.2～112μg·mL^(-1)、10.02～100.2μg·mL^(-1)、10.32～103.2μg·mL^(-1)内线性关系良好,精密度、重复性、稳定性试验RSD均<1.8%,加样回收率分别为98.34%～101.77%(RSD=1.28%,n=6)、98.69%～101.36%(RSD=1.01%,n=6)、98.46%～101.06%(RSD=0.92%,n=6)、98.67%～101.33%(RSD=1.17%,n=6)、98.43%～100.79%(RSD=0.92%,n=6)。结论本研究建立的质量标准方法准确、简便,可用于川菊止痛胶囊的质量控制,且所建立的菊花、柴胡薄层鉴别方法可供其他含有二药的复方标准建立作参考。

OBJECTIVE To establish the quality standard for Chuanju Zhitong capsule. METHODS TLC was used to qualitatively identify the compound Bupleuri Radix and Chrysanthemum Flos, respectively. HPLC was used to determine the contents of baicalin, baicalein, wogonoside, wogonin and liquiritin. The determination was performed on Kromasil 100-5C18(250 mm×4.6 mm, 5 μm) column with mobile phase consisted of acetonitrile-0.05% phosphoric acid, gradient elution at flow rate of 1.0 mL·min-1;the detection wavlength was set at 280 nm;the injection volume was 10 μL. RESULTS TLC spots were clear and well separated without negative interference. The linear range of baicalin, baicalein, wogonoside, wogonin and liquiritin were 10.7-107 μg·mL-1, 12.12-121.2 μg·mL-1, 11.2-112 μg·mL-1, 10.02-100.2 μg·mL-1 and 10.32-103.2 μg·mL-1. RSDs of precision, stability and reproducibility tests were <1.8%. The recoveries were 98.34%-101.77%(RSD=1.28%, n=6),98.69%-101.36%(RSD=1.01%, n=6), 98.46%-101.06%(RSD=0.92%, n=6), 98.67%-101.33%(RSD=1.17%, n=6), 98.43%-100.79%(RSD=0.92%, n=6), respectively. CONCLUSION The established quality standard method is accurate and simple, can be used for the quality control of Chuanju Zhitong capsule, the TLC of Chrysanthemum Flos and Bupleuri Radix can be used for other Chinese herbal compound.