三步碱沉法制备地榆总皂苷的工艺优选

发布时间：2018-09-19 08:21

【摘要】：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。
[Abstract]:OBJECTIVE:To optimize the extraction and purification conditions of total saponins from Sanguisorba officinalis by orthogonal test and three-step precipitation method.METHODS:The content of saponins from Sanguisorba officinalis was determined by HPLC-ELSD,the mobile phase was gradient elution with methanol-acetonitrile(1:1)-water,the drift temperature of evaporative light scattering detector was 100 C,the gas flow rate was 3.0 L.min-1.The transfer rate of saponins from Sanguisorba officinalis- The extraction process of total saponins from Sanguisorba officinalis was optimized by orthogonal test, and the tannin removal rate and the content of saponins from Sanguisorba officinalis L. were used as evaluation indexes. The purification process was optimized by single factor test. The supernatant was adjusted by 10% NaOH solution for 24 hours, centrifuged and dried at 70 C for 30 minutes. The ethanol was recovered by 30 times of anhydrous ethanol for 30 minutes. The purity of total saponins was 91.32%. The extraction and purification process of total saponins is simple and stable, and the yield of total saponins is high. It is suitable for industrial production.
【作者单位】：成都中医药大学药学院中药材标准化教育部重点实验室四川省中药资源系统研究与开发利用重点实验室——省部共建国家重点实验室培育基地;江西中医药大学现代中药制剂教育部重点实验室;
【基金】：国家自然科学基金项目(81373976) 国家“重大新药创制”科技重大专项(2013ZX09103002-013)
【分类号】：R283.6

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