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目的:通过正交试验与三步沉淀法优选地榆总皂苷的提取与纯化工艺条件。方法:采用HPLC-ELSD测定地榆皂苷-Ⅰ的含量,流动相[甲醇-乙腈(1∶1)]-水梯度洗脱,蒸发光散射检测器的漂移温度100℃,气体流速3.0 L·min-1。以地榆皂苷-Ⅰ转移率为指标,通过正交试验优选地榆总皂苷的提取工艺;采用三步碱沉法,以鞣质清除率与地榆皂苷-Ⅰ含量为评价指标,通过单因素试验优选纯化工艺。结果:地榆总皂苷最佳工艺条件为加8倍量70%乙醇回流提取2次,每次1.5 h,提取液加10%氢氧化钠溶液调p H 12~14,静置12 h,离心去沉淀,上清液用10%氢氧化钠溶液调p H 12~13,静置24 h,离心,沉淀于70℃减压干燥至干,用30倍量无水乙醇回流30 min,减压回收乙醇至有固形物析出,固形物减压干燥12 h。地榆总皂苷纯度91.32%。结论:优选的地榆总皂苷提取纯化工艺路线简单、稳定,制备的地榆总皂苷得率、纯度高,适合工业化生产。
OBJECTIVE: To optimize the extraction and purification of total saponins from elm by orthogonal experiment and three-step precipitation method. Methods: The content of saponin-I was determined by HPLC-ELSD. The mobile phase consisted of gradient elution of methanol-acetonitrile (1: 1) -water. The evaporation temperature of evaporative light scattering detector was 100 ℃ and gas flow rate was 3.0 L · min -1. Saponins-Ⅰ transfer rate as an indicator, through orthogonal test, preferably elm total saponin extraction process; using three-step alkali precipitation, tannin clearance and Sapogenin-Ⅰ content as the evaluation index through a single factor The test is preferably a purification process. Results: The optimum conditions of total saponins of Burnet were extracted with 8 times the amount of 70% ethanol by refluxing for 2 times, each time being 1.5 h. The extract and 10% sodium hydroxide solution were adjusted to pH 12-14 and allowed to stand for 12 h. To precipitate, the supernatant with 10% sodium hydroxide solution p H 12 ~ 13, allowed to stand 24 h, centrifuged, the precipitate was dried at 70 ° C under reduced pressure and dried with 30 times the amount of absolute ethanol reflux for 30 min, depressurized Recovery of ethanol to a solid precipitation, solid vacuum drying 12 h. Burnet total saponin purity of 91.32%. Conclusion: The optimal extraction process of total saponins from Burnet is simple and stable. The total saponins from Burnet are superior in purity and purity and suitable for industrialized production.