目的 明确黄明胶、蜂蜜混合辅料膏方制备工艺的最佳参数。方法 以润肠通便方为模型药物,以膏方的黄明胶、蜂蜜使用量以及成品膏相对密度为考察因素,膏方的成型性和指纹图谱为控制指标,运用星点设计-效应面法优化膏方制备工艺。结果 膏方提取工艺:加水6倍量,浸泡0.5 h,煎煮3次,每次1 h,其中首次提取加水8倍量。膏方指纹图谱主要色谱条件:流动相为乙腈-0.1%磷酸水溶液,梯度洗脱:0～5 min,10%乙腈;5～15 min,10%～35%乙腈;15～30 min,35%～85%乙腈;检测波长238、280 nm。膏方指纹图谱共发现12个共有峰,指认7号峰为和厚朴酚(参比峰,S),各个共有峰相对保留时间和相对峰面积的精密度、重复性、稳定性的RSD值均小于3%。膏方制备工艺为黄明胶使用量8%～12%、蜂蜜使用量22%～28%、成品膏相对密度1.20～1.25。膏方制备放大试验验证,偏差绝对值均小于3%。结论 该方法可以保证膏方具有较好的成型性,以及化学成分相对较高的转移率。

Objective To clarify the optimum conditions for the preparation of mixed materials of oxhide gelatin and honey. Methods Using the dosage of oxhide gelatin and honey as well as the relative density of refined cream as factors, and the paste forming and fingerprints as control indexes, the central composite design and response surface method was used to optimize the paste preparation process. Results The extraction process was as follows: 6 times of water amount, soaked for 0.5 h, extracted for three times and each time was 1 h, which was 8 times of water for the first time. The main chromatographic conditions of paste fingerprints were as follows: Mobile phase was acetonitrile-0.1% phosphoric acid gradient [acetonitrile: 10% (0—5 min); 10%—35% (5—15 min); 35%—85% (15—30 min)], and detection wavelengths were 238 and 280 nm. Paste fingerprint: 12 common peaks were found, and the peak No. 7 was identified on honokiol. The RSD values of precision, reproducibility, and stability of each peak relative retention time and relative peak area precision were all less than 3%. The best conditions in the preparation process of cream were as follows: oxhide gelatin (8%—12%), honey (22%—28%), the refined cream and relative density (1.20—1.25). The absolute value of the deviation was less than 3% of paste preparation amplification experiments. Conclusion This method can be used to ensure that the paste had good formability, and the chemical composition is relatively high.

国家临床重点专科(中医专业)建设项目——临床药学