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目的:建立消渴丸的HPLC特征图谱分析方法。方法:采用高效液相色谱法对20批消渴丸样品进行分析。色谱条件:Welch Materials XB-C18色谱柱(4.6 mm×260 mm,5μm);流动相为甲醇-0.02%甲酸水溶液;流速为1.0 mL·min-1;以葛根素为参照峰,检测波长为280 nm。结果:采用《中药色谱指纹图谱相似度评价系统2.0版》分析了20批消渴丸样品,确定了12个共有峰,20批消渴丸样品的相似度均在0.98以上;利用对照品的保留时间及紫外光谱比较,确认了其中的8个共有峰,分别为3’-羟基葛根素(3号峰)、葛根素(4号峰)、3’-甲氧基葛根素(5号峰)、大豆苷元-8-C-芹糖基-(1#6)-葡萄糖苷(6号峰)、大豆苷(7号峰)、大豆素(10号峰)、五味子酯甲(11号峰)及五味子甲素(12号峰)。所归属的色谱峰峰面积占总峰面积的80%,占共有峰面积的85%。此外,通过比较消渴丸样品与原药材的HPLCDAD色谱图,明确了3~7号共有峰来源于葛根,11~12号共有峰来源于南五味子。结论:该方法符合方法学验证要求,可检测消渴丸中的多种成分,所构建的特征图谱能较全面、准确地评价消渴丸质量的均一性,可为消渴丸的整体质量评价提供参考。
Objective: To establish the method of HPLC profile analysis of Xiaoke Pills. Methods: Twenty batches of Xiaoke Pill samples were analyzed by high performance liquid chromatography. Chromatographic conditions: Welch Materials XB-C18 column (4.6 mm × 260 mm, 5μm); mobile phase of methanol -0.02% aqueous solution of formic acid; flow rate of 1.0 mL · min-1; puerarin as a reference peak, the detection wavelength was 280 nm. RESULTS: Twenty batches of Xiaoke Pill samples were analyzed using the “Chinese Medicines Chromatographic Fingerprint Similarity Evaluation System Version 2.0”, the 12 common peaks were identified and the similarity of 20 batches of Xiaoke Pills samples were all above 0.98. Using the retention of the reference substance Time and UV spectra, 8 common peaks were identified, which were 3’-hydroxy puerarin (No.3), puerarin (No.4) and 3’-methoxy puerarin , Daidzein -8-C-glycosyl- (1 # 6) -glucoside (peak 6), daidzin (peak 7), daidzein (peak 10) ) And Schisandra A (peak 12). The attributable peak area of the chromatographic peak area of 80%, accounting for 85% of the total peak area. In addition, by comparing HPLCDAD chromatogram of Xiaoke Pill sample and original medicinal material, it is clear that the common peak number 3 to 7 is from Pueraria lobata, and the common peak from 11 to 12 is from Schisandra chinensis. Conclusion: The method meets the requirements of methodological verification and can detect many components of Xiaoke Pill. The constructed characteristic map can evaluate the quality uniformity of Xiaoke Pills more comprehensively and accurately, and can be used to evaluate the overall quality of Xiaoke Pills for reference.