消炎利胆片中4-甲氧基-5-羟基-铁屎米酮的定性定量方法研究  

Qualitative and quantitative analysis of 4- methoxy- 5- hydroxycanthin- 6- one in Xiaoyan Lidan tablets

作　　者：杨娜[1] 郑程[1] 郭夫江[1] 王瑞[1] 王峥涛[2,3] 

机构地区：[1]上海中医药大学中药学院,上海201203 [2]上海中医药大学中药研究所,中药标准化教育部重点实验室,中药新资源与质量标准综合评价国家中医药管理局重点研究室,上海201203 [3]上海中药标准化研究中心,上海201203

出　　处：《药物分析杂志》2013年第12期2166-2170,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委员会“国家药品标准提高暨2015版药典科研任务”项目

摘　　要：目的：建立消炎利胆片中苦木的有效成分4-甲氧基-5-羟基-铁屎米酮的定性定量分析方法。方法：采用薄层色谱法进行定性鉴别，薄层板为Pre-coated TLC-plates SIL G-25 UV254，展开剂为丙酮-三氯甲烷-甲醇-甲酸（1：13：0.1：0.1），于紫外光灯（254 nm）下检视；采用反相高效液相色谱法测定含量，色谱柱为CAPCELL PAK-C18 MGS5（250 mm×4.6 mm，5 μm），流动相为乙腈-0.02%磷酸水溶液（28：72），流速1.0 mL·min-1，检测波长254 nm，柱温30 ℃。结果：在薄层色谱中可检出4-甲氧基-5-羟基-铁屎米酮，斑点清晰，分离度好；4-甲氧基-5-羟基-铁屎米酮进样量在0.0091~0.5810 μg范围内与峰面积呈良好的线性（r=1.000），平均回收率（n=9）为98.7%，样品含量范围为0.0166~0.5767 mg·片-1。结论：所建立的方法简单灵敏，准确可靠，重复性好，可用于消炎利胆片的质量控制，为消炎利胆片2015年版中国药典质量标准研究奠定基础。Objective： To establish qualitative and quantitative methods for the quality evaluation of 4-methoxy-5-hydroxycanthin-6-one in Xiaoyan Lidan tablets. Methods： The component in Xiaoyan Lidan tablets was identified and determined by TLC and HPLC,respectively.Qualitative analysis was performed on the thin-layer pre-coated TLC-plates SIL G-25 UV254,with acetone-trichloromethane-methanol-formic acid（1：13：0.1：0.1）as the developing solvent,and the detection was performed at 254 nm with a UV lamp.Quantitative analysis was performed on CAPCELL PAK-C18 MGS5（4.6 mm×250 mm,5 μm）.The mobile phase was acetonitrile-water-0.02% phosphoric（28：72）at the flow rate of 1.0 mL·min-1,the detection wavelength was 254 nm and the column temperature was 30 ℃. Results： 4-methoxy-5-hydroxycanthin-6-one could be detected by TLC,and the spots were clear,with high clarity. Calibration curve showed good linear regression（r=1.000）within test ranges of 0.0091-0.5810 μg.The average recovery（n=9）was 98.7%,and the range of contents in the samples were 0.0166-0.5767 mg per tablet. Conclusion： The methods developed are sensitive,reliable and useful for the analysis of samples purchased from different areas and can be used for the quality control of Xiaoyan Lidan tablets.

关 键 词：消炎利胆片 4-甲氧基-5-羟基-铁屎米酮 薄层色谱法 高效液相色谱法 中成药 质量控制 质量标准完善 

分 类 号：R917[医药卫生—药物分析学]