覆盆子生药粉湿热灭菌工艺优化及不同灭菌方式对质量影响研究

Optimization of moist heat sterilization technology for Rubus chingii and quality impact research for different sterilization methods

目的 通过多指标正交试验优选覆盆子生药粉最佳湿热灭菌工艺,对比不同灭菌方式对覆盆子生药粉的灭菌效果及质量的影响。方法 以山柰酚3-O-芸香糖苷、鞣花酸的含量和灭菌率的综合评分为指标,采用层次分析(AHP)法、指标重复性相关(CRITIC)法和AHP-CRITIC混合加权法确定各指标权重系数,结合正交试验筛选覆盆子湿热灭菌工艺中灭菌时间、灭菌温度和物料厚度,优化覆盆子灭菌工艺参数;通过微生物限度检测,生药粉椴树苷鉴别,水分、总灰分、酸不溶灰分、浸出物、山柰酚3-O-芸香糖苷和糅花酸含量检测,指纹图谱检测,对比采用湿热灭菌、辐照灭菌、干热灭菌和乙醇灭菌法对覆盆子生药灭菌效果和质量的影响。结果 AHP-CRITIC混合加权法较AHP法和CRITIC法更为科学、合理,按照其确定的权重系数进行综合评价确定的覆盆子最佳湿热灭菌工艺条件为灭菌时间15 min、灭菌温度115℃、物料厚度5 mm;各灭菌样品的微生物限度检查等均符合药典规定,与未灭菌生药粉相比,山柰酚3-O-芸香糖苷经乙醇灭菌与干热灭菌后含量降低,糅花酸经干热灭菌后含量增加;指纹图谱结果 显示,干热灭菌与未灭菌相比相似度较低,辐照灭菌、湿热灭菌与未灭菌相比相似度较高。结论 湿热灭菌法与其他灭菌方法 相比,可在较低温度、更短时间得到符合规定的覆盆子生药粉,且优选得到的灭菌工艺稳定可行、重复性好。

Objective To optimize the sterilization process of crude drug power of Rubus chingii through multi-index orthogonal experiment, compare the effect of different sterilization methods on the sterilization effect and quality of crude drug power of Rubus chingii. Methods With the content of kaempferol 3-O-rutinoside, ellagic acid and the sterilization rate as comprehensive evaluation indexes, weight coefficient of indicators were determined by AHP, CRITIC and AHP-CRITIC mixed weighting method, L9(34)orthogonal test was used to sterilization time, sterilization temperature and material thickness, in sterilization process of Rubus chingii, optimizing process parameters of sterilization. The sterilization effect and quality of crude drug power of Rubus chingii before and after sterilization were compared by moist heat sterilization, irradiation sterilization, dry heat sterilization and ethanol sterilization. Results The weight coefficient determined by AHP-CRITIC mixed weighting method was the most reasonable. The optimal extraction technology was sterilization time 30 min, sterilization temperature 115 ℃ and material thickness 5 mm. The microbial limit inspection of each sterilized sample complies with the pharmacopoeia regulations. Compared with the unsterilized crude drug powder, the content of kaempferol 3-O-rutinoside was reduced after ethanol sterilization and dry heat sterilization. The content increased after sterilization. The fingerprint results showed that the similarity of dry heat sterilization was lower than that of non-sterilized, and the similarity of radiation sterilization and moist heat sterilization was higher than that of non-sterilized.Conclusion Compared with other sterilization methods, the moist heat sterilization method can obtain the crude drug power of Rubus chingii that meets the requirements at a lower temperature and in a shorter time. The preferably obtained sterilization process is stable, feasible, and reproducible.