高效液相色谱法同时测定降脂通便胶囊中5种蒽醌  

Simultaneous determination of five anthraquinones in Jiangzhi Tongbian Capsules by high performance liquid chromatography

作　　者：汪明志 钱叶飞 张超 WANG Mingzhi;QIAN Yefei;ZHANG Chao(Suzhou Institute for Drug Control,Suzhou 215204,China)

机构地区：[1]苏州市药品检验检测研究中心,江苏苏州215204

出　　处：《化学分析计量》2025年第1期21-25,共5页Chemical Analysis And Meterage

基　　金：江苏省药品监督管理局科研计划课题(202128)。

摘　　要：建立反相高效液相色谱法同时测定降脂通便胶囊中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚5种蒽醌含量。样品用甲醇回流提取后用硫酸水解,用三氯甲烷萃取,以Sepax Bio-C_(18)(250 mm×4.6 mm,5μm)色谱柱分离,以甲醇-乙腈-0.1%磷酸溶液(体积比为23∶42∶35)为流动相,流量为1 mL/min,检测波长为254 nm,柱温为35℃。5种蒽醌的质量分别在0.0588~0.3528、0.7036~4.2216、0.0672~0.4032、0.0836~0.501、0.1058~0.6348μg范围内与色谱峰面积呈良好的线性关系,相关系数均不小于0.9998,方法检出限为0.0015~0.0042μg/mL,定量限为0.0047~0.0133μg/mL。样品加标平均回收率为96.47%~98.35%,测定结果的相对标准偏差为1.1%~2.0%(n=6)。该方法满足降脂通便胶囊中5种蒽醌成分的测定要求,可以为降脂通便胶囊的质量控制提供一定的技术参考。A method for simultaneous determination of five anthraquinones,including aloe emodin,rhein,emodin,chrysopranol,and emodin methylether,in Jiangzhi Tongbian Capsules by a reverse phase high performance liquid chromatography was established.The sample was extracted by refluxing with methanol,hydrolyzed with sulfuric acid,and extracted with trichloromethane.Sepax Bio-C_(18)(250 mm×4.6 mm,5μm)chromatographic column was used for separation,with methanol-acetonitrile-0.1%phosphoric acid(volume ratio was 23∶42∶35)as the mobile phase,flow rate of 1 mL/min,detection wavelength of 254 nm,and column temperature of 35℃.The mass of the five anthraquinone had a good linear relationship with the chromatographic peak area in the ranges of 0.0588-0.3528,0.7036-4.2216,0.0672-0.4032,0.0836-0.501,0.1058-0.6348μg,respectively.The correlation coefficients were not less than 0.9998.The detection limits of the method were 0.0015-0.0042μg/mL,and the quantification limits were 0.0047-0.0133μg/mL.The average recoveries of sample spiked were 96.47%-98.35%,and the relative standard deviations of the determination results were 1.1%-2.0%(n=6).This method meets the requirements for the determination of five anthraquinone components in Jiangzhi Tongbian Capsules,which can provide a certain technical reference for the quality control of Jiangzhi Tongbian capsules.

关 键 词：高效液相色谱法 降脂通便胶囊 蒽醌 

分 类 号：O657.7[理学—分析化学]