[关键词]
[摘要]
目的 建立用HPLC波长切换法同时测定大黄利胆片中10个活性成分没食子酸、5-羟甲基糠醛、柯里拉京、对羟基苯甲醛、鞣花酸、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚含量的方法,并结合统计学分析对其质量进行评价。方法 采用Phenomenex Kinetex C18色谱柱,柱温为30℃,以甲醇-0.15%磷酸水溶液为流动相梯度洗脱,体积流量为1 mL/min,检测波长分别为265.0 nm(0~5.8 min,检测没食子酸)、283.9 nm(5.8~7 min,检测5-羟甲基糠醛)、222.2(7~18 min,检测柯里拉京、对羟基苯甲醛)、256.7 nm(18~74 min,检测鞣花酸、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚);用SPSS 21软件对10批药中成分含量进行统计学分析。结果 10个成分在各自质量浓度范围内线性关系良好(r>0.998 0),平均加样回收率98.45%~100.12%,RSD为0.80%~2.51%;含量分别为没食子酸8.371~11.438 mg/片、5-羟甲基糠醛0.046~0.087 mg/片、柯里拉京0.721~2.094 mg/片、对羟基苯甲醛0.034~0.065 mg/片、鞣花酸1.736~1.996 mg/片、芦荟大黄素0.337~0.440 mg/片、大黄酸1.636~2.562 mg/片、大黄素0.602~0.846 mg/片、大黄酚0.388~0.566 mg/片、大黄素甲醚0.621~0.781 mg/片;10批样品质量基本一致。结论 该方法简单准确,可用于大黄利胆片的质量控制。
[Key word]
[Abstract]
Objective A method for simultaneous determination of 10 active ingredients in Dahuang Lidan Tablets (DLP) by HPLC wavelength switching method was established, and its quality was evaluated by statistical analysis. Methods A Phenomenex Kinetex C18 column was used with a column temperature of 30℃ and a mobile phase gradient of methanol-0.15% phosphoric acid. The flow rate was 1 mL/min and the detection wavelengths were 265.0 nm (0-5.8 min, gallic acid), 283.9 nm (5.8-7 min, 5-hydroxymethyl furfural), 222.2 nm (7-18 min, corilagin, p-hydroxybenzaldehyde), 256.7 nm (18-74 min, ellagic acid, aloe-emodin, rhein, emodin, chrysophanol, emodin methyl ether), respectively. Statistical analysis of the content of components in 10 batches of drugs was performed using SPSS 21 Software. Results The linearity of 10 components in the respective mass concentration ranges was good (r > 0.998 0), the average sample recovery was in the range of 98.45%-100.12%, and the RSD was in the range of 0.80%-2.51%. The content of 10 components was as follow:gallic acid (8.371-11.438 mg/tablet), 5-hydroxymethylfurfural (0.046-0.087 mg/tablet), corilagin (0.721-2.094 mg/tablet), p-hydroxybenzaldehyde (0.034-0.065 mg/tablet), ellagic acid (1.736-1.996 mg/tablet), aloe-emodin (0.337-0.440 mg/tablet), rhein (1.636-2.562 mg/tablet), emodin (0.602-0.846 mg/tablet), chrysophanol (0.388-0.566 mg/tablet) and emodin methyl ether (0.621-0.781 mg/tablet). The quality of the 10 batches of samples was basically the same. Conclusion This method is simple and accurate and can be used for the quality control of DLP.
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[基金项目]
河南省科技厅科技攻关计划(152102310102);河南中医药大学研究生创新创业团队项目(2018CXCY11)