目的 优选地龙活性组分的冻干工艺.方法 采用单因素试验结合Box-Behnken响应面法,以冻干率为指标,考察1次升华温度、升华时间、解析干燥温度、解析干燥时间等因素对冻干工艺的影响,优化地龙活性组分的冻干工艺,采用HPLC法,测定优化后工艺样品的指纹图谱,并比较其与地龙药材指纹图谱相似度,确定最佳冻干工艺.结果 确定地龙活性组分的最佳冻干工艺条件:预冻温度-26.5 ℃,预冻4 h,升华干燥温度-20 ℃、升华时间7 h、解析干燥温度30 ℃、解析干燥时间3.5 h,冻干率为96.55%,与对照药材的氨基酸指纹图谱相似度均大于0.9.结论 Box-Behnken响应面法用于地龙活性组分冻干工艺条件的优选是可行的,模型预测效果较好,优化工艺具备可行性.

Objective To optimize the technology of freeze-dried powder of various fractions from lumbricus(Pheretima) by Box-Behnken design and response surface method. Methods Using single factor experiment with Box-Behnken response surface method, freeze-dried rate as the index, the effects of sublimation temperature, sublimation time, analytical drying temperature, and drying time on the freeze-drying process were observed; The freeze-drying process of the active components in lumbricus was optimized; Using HPLC method, the fingerprint of the sample by the optimized technology was investigated, and the similarity of fingerprint was compared with the earthworm medicine, and the optimum freeze-drying process was obtained. Results The best freeze-drying process conditions of active components in lumbricus were as follows: frozen temperature of -26.5 ℃, precool for 4 h, sublimation drying temperature of -20 ℃, sublimation time of 7 h, analytical drying temperature of 30 ℃, analytical drying time of 3.5 h, freeze-dried rate of 96.55%, and compared with medicinal materials of amino acid, the similarities of fingerprint were both greater than 0.9. Conclusion Box-Behnken response surface method is used for the freeze-drying process conditions of active components in the lumbricus, the optimization is feasible, the effect of model is good, and this optimization process has the feasibility.

国家"十二五"重大新药创制科技重大专项资助项目(2014ZX09201-022-03);湖北省重大科技创新专项资助项目(2013ACC005)