目的 建立桃核承气汤（Taohe Chengqi Decoction，TCD）物质基准的HPLC特征图谱及指标成分含量测定方法，阐明TCD物质基准的关键质量属性，构建其质量控制体系。方法 特征图谱1，色谱柱为Diamonsil钻石二代C₁₈色谱柱（250 mm×4.6 mm，5 μm），甲醇-0.1%磷酸水溶液为流动相，体积流量为1.0 mL/min，梯度洗脱，进样量为10 μL，柱温30 ℃，检测波长为254 nm；特征图谱2，色谱柱为Diamonsil钻石一代C₁₈色谱柱（250 mm×4.6 mm，5 μm），甲醇-0.2%磷酸水溶液为流动相，体积流量为1.0 mL/min，梯度洗脱，进样量为10 μL，柱温35 ℃，检测波长为210 nm。结果 根据方中成分的极性差异，建立2张特征图谱，结果显示，15批TCD物质基准相似度分别为0.928～0.992和0.809～0.995，共确定32个特征峰，并指认苦杏仁苷、甘草苷、甘草酸铵、芦荟大黄素、大黄酸5个共有成分。15批TCD物质基准的平均出膏率为19.10%，苦杏仁苷、甘草酸铵、桂皮醛、芦荟大黄素、大黄酸的质量分数分别为2.650～7.318、3.563～17.486、0.013～0.128、0.034～0.215、0.930～3.582 mg/g。结论 为TCD物质基准的质量控制和复方制剂开发提供科学依据。

Objective To establish the HPLC characteristic chromatogram and content determination method of index components in Taohe Chengqi Decoction (TCD) substance benchmarks, which clarified the critical quality attributes and constructed the quality control system. Methods For characteristic chromatogram 1, the separation was performed on the Diamonsil diamond second-generation C₁₈ column (250 mm×4.6 mm, 5 μm) at 30 ℃. The mobile phase consisted of methanol and water with 0.1% phosphoric acid at a flow rate of 1.0 mL/min. The detection wavelength was 254 nm; Characteristic chromatographic 2 analysis was performed using the Diamonsil diamond first-generation C₁₈ column (250 mm×4.6 mm, 5 μm). Methanol and 0.2% phosphoric acid aqueous solution were utilized as the mobile phases. The flow rate was set at 1.0 mL/min using a gradient program. The temperature of the column was maintained at 35 ℃, and the signal was detected at 210 nm. For these two methods, the injection volume of the standard and sample was kept as 10 µL. Results According to polarity differences among these components of TCD, two HPLC characteristic chromatograms were established. The similarities for the two HPLC characteristic chromatograms of 15 batches of substance benchmarks of TCD were 0.928—0.992 and 0.809—0.995, respectively. A total of 32 characteristic peaks were identified and five common components were identified as amygdalin, glycyrrhizin, ammonium glycyrrhizinate, aloe-emodin, and rhein. The average dry extract yield of 15 batches of TCD was 19.10%. The contents of amygdalin, ammonium glycyrrhizinate, cinnamaldehyde, aloe-emodin and rhein were 2.650—7.318, 3.563—17.486, 0.013—0.128, 0.034—0.215, 0.930—3.582 mg/g, respectively. Conclusion This study could provide scientific basis for the quality control of substance benchmarks and the development of compound preparations of TCD.

R286.02

国家自然科学基金面上项目（81673562）