目的 通過多指標正交試驗優(yōu)選覆盆子生藥粉最佳濕熱滅菌工藝，對比不同滅菌方式對覆盆子生藥粉的滅菌效果及質(zhì)量的影響。方法 以山柰酚3-O-蕓香糖苷、鞣花酸的含量和滅菌率的綜合評分為指標，采用層次分析（AHP）法、指標重復(fù)性相關(guān)（CRITIC）法和AHP-CRITIC混合加權(quán)法確定各指標權(quán)重系數(shù)，結(jié)合正交試驗篩選覆盆子濕熱滅菌工藝中滅菌時間、滅菌溫度和物料厚度，優(yōu)化覆盆子滅菌工藝參數(shù)；通過微生物限度檢測，生藥粉椴樹苷鑒別，水分、總灰分、酸不溶灰分、浸出物、山柰酚3-O-蕓香糖苷和糅花酸含量檢測，指紋圖譜檢測，對比采用濕熱滅菌、輻照滅菌、干熱滅菌和乙醇滅菌法對覆盆子生藥滅菌效果和質(zhì)量的影響。結(jié)果 AHP-CRITIC混合加權(quán)法較AHP法和CRITIC法更為科學(xué)、合理，按照其確定的權(quán)重系數(shù)進行綜合評價確定的覆盆子最佳濕熱滅菌工藝條件為滅菌時間15 min、滅菌溫度115℃、物料厚度5 mm；各滅菌樣品的微生物限度檢查等均符合藥典規(guī)定，與未滅菌生藥粉相比，山柰酚3-O-蕓香糖苷經(jīng)乙醇滅菌與干熱滅菌后含量降低，糅花酸經(jīng)干熱滅菌后含量增加；指紋圖譜結(jié)果顯示，干熱滅菌與未滅菌相比相似度較低，輻照滅菌、濕熱滅菌與未滅菌相比相似度較高。結(jié)論 濕熱滅菌法與其他滅菌方法相比，可在較低溫度、更短時間得到符合規(guī)定的覆盆子生藥粉，且優(yōu)選得到的滅菌工藝穩(wěn)定可行、重復(fù)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.

R282.4

國家重點研發(fā)計劃-中藥口服制劑先進制造關(guān)鍵技術(shù)與示范研究(2019YFC1711200);山東省重點研發(fā)計劃(重大科技創(chuàng)新工程)(2020CXGC010505)