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目的采用HPLC同时测定四季三黄片中芦荟大黄素、黄芩苷、黄柏酮和西红花苷-Ⅰ的含量。方法采用Welch Topsil-C18色谱柱(4.6 mm×250 mm,4μm);流动相:甲醇-0.2%磷酸水溶液;梯度洗脱;检测波长分别为254 nm(芦荟大黄素、黄芩苷、黄柏酮)和440 nm(西红花苷-Ⅰ);流速:1.0 m L·min~(-1);柱温:30℃。结果芦荟大黄素、黄芩苷、黄柏酮和西红花苷-Ⅰ线性范围分别为0.079 10~1.582μg·m L~(-1)(r=0.999 5),0.167 5~3.350μg·m L~(-1)(r=0.999 8),0.097 92~1.958μg·m L~(-1)(r=0.999 7)和0.033 57~0.671 5μg·m L~(-1)(r=0.999 4),平均加样回收率分别为95.9%(RSD=0.7%),97.5%(RSD=0.8),96.4%(RSD=1.0%),95.5%(RSD=1.3%)。结论该方法简便、准确、专属性强、重复性好,可用于四季三黄片中芦荟大黄素、黄芩苷、黄柏酮和西红花苷-Ⅰ的定量分析。
OBJECTIVE To determine the contents of aloe-emodin, baicalin, chlortetone and crocin-Ⅰ in Shiji San Huang tablets simultaneously by HPLC. The method was performed on a Welch Topsil-C18 column (4.6 mm × 250 mm, 4 μm). The mobile phase consisted of methanol-0.2% phosphoric acid solution and gradient elution. The detection wavelength was 254 nm 440 nm (crocin-I); flow rate: 1.0 m L · min -1; column temperature: 30 ℃. Results The linear range of aloe-emodin, baicalin, vinorelbine and crocin-I were 0.079 10-1.582 μg · mL -1 (r = 0.999 5), 0.167 5-3.350 μg · m L -1 (R = 0.999 8), 0.097 92 ~ 1.958 μg · m L -1 (r = 0.999 7) and 0.033 57 ~ 0.671 5 μg · m L -1 (r = 0.999 4) The average recoveries were 95.9% (RSD = 0.7%), 97.5% (RSD = 0.8), 96.4% (RSD = 1.0%) and 95.5% (RSD = 1.3%), respectively. Conclusion The method is simple, accurate, specific and reproducible. It can be used for the quantitative analysis of aloe-emodin, baicalin, chlorton and crocin-Ⅰ in Siji Sanhuang tablets.