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目的采用微滤与微波真空干燥联用技术,研究提高三七三醇皂苷(PTS)质量和产量的工业化生产。方法以静态饱和吸附量、PTS纯度、收率、有效成分转移率与指纹图谱为主要评价指标,考察了微滤对PTS与大孔吸附树脂的影响,进行微滤工艺L9(34)正交试验,经多批次验证与评价,确定微滤技术的可行性;以干燥PTS纯度、水分、损耗率、有效成分转移率和指纹图谱为评价指标,对干燥工艺进行筛选,进行L9(34)正交试验,经多批次验证与评价,确定微波真空干燥的可行性。结果微滤工艺,可改善产物性状、提高PTS纯度、延长树脂的再生周期、提高卫生学质量,指纹图谱相似度可大于0.99(n=5);微波真空干燥使PTS损耗率由4%～5%降低至0.2%～0.5%,指纹图谱相似度可大于0.99(n=5)。结论采用微滤与微波真空干燥联用技术能大幅度提高PTS工业化生产的质量及产量,工艺稳定,重复性好。
Objective To improve the quality and yield of PTS by using microfiltration and microwave vacuum drying technology. Methods The static adsorption capacity, PTS purity, yield, active ingredient transfer rate and fingerprint were used as the main evaluation indexes. The effects of microfiltration on PTS and macroporous resin were investigated. The orthogonal experiment L9 (34) , And the feasibility of microfiltration was confirmed through batch verification and evaluation. The drying process was screened by the purity, moisture, wastage rate, active ingredient transfer rate and fingerprint of dry PTS, and L9 (34) positive To test, after multiple batches of validation and evaluation to determine the feasibility of microwave vacuum drying. Results Microfiltration process can improve product traits, improve the purity of PTS, prolong the regeneration cycle of the resin and improve the hygiene quality. The similarity of fingerprint can be greater than 0.99 (n = 5). Microwave vacuum drying reduced the PTS loss from 4% to 5 % To 0.2% ~ 0.5%, fingerprint similarity greater than 0.99 (n = 5). Conclusion The combination of microfiltration and microwave vacuum drying can greatly improve the quality and yield of PTS industrialized production with stable process and good repeatability.