摘要
Abstract
Objective To establish an ultra-high performance liquid chromatography(UPLC)method for simultaneous determination of 11 chemical components in Siji Sanhuang Pills,and to evaluate the quality of the preparations.Methods The chromatographic column was the Waters HSS T3 column(100 mm×2.1 mm,1.8 µm),the mobile phase was 0.1% trifluoroacetic acid aqueous solution-acetonitrile(gradient elution),the flow rate was 0.3 mL/min,the detection wavelength was 250 nm,the column temperature was 30℃,and the injection volume was 1 µL.The established method was used to determine the contents of geniposide,baicalin,wogonoside,berberine hydrochloride,baicalein,wogonin,aloe-emodin,rhein,emodin,chrysophanol and physcion in 25 batches of samples from two manufacturing enterprises.The overall quality of the samples was evaluated by the cluster analysis(CA)and partial least square-discriminant analysis(PLS-DA).Results The linear ranges of 11 components were 0.080 6-8.06 µg,0.194 0-19.40 µg,0.049 4-4.94 µg,0.088 9-8.89 µg,0.030 4-3.04 µg,0.014 2-1.42 µg,0.017 9-1.79 µg,0.016 94-1.69 µg,0.020 0-2.00 µg,0.025 9-2.59 µg,0.009 18-0.92 µg(r≥0.999 5)respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0% .The average recovery rate of 11 components was in the range of 96.90%-102.01%,with the RSDs in the range of 0.52%-2.58% (n=9).The overall quality of samples from the same manufacturer was consistent,and that was distinct between different manufacturers.The main components that induced quality differences were baicalin,rhein,wogonoside,baicalein and wogonin.Conclusion The established method is easy,accurate and reliable,which can be used to determine the contents of 11 chemical components in Siji Sanhuang Pills and evaluate their quality.Relevant enterprises should focus on the contents of the above components especially baicalin and rhein in the preparations to ensure the therapeutic effect of the products.关键词
四季三黄丸/超高效液相色谱法/聚类分析/偏最小二乘-判别分析/黄芩苷/大黄酸/汉黄芩苷/质量评价Key words
Siji Sanhuang Pills/UPLC/cluster analysis/partial least square-discriminant analysis/baicalin/rhein/wogonoside/quality evaluation分类
医药卫生
