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

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.