Optimization of Three-step Alkali Precipitation Method for Preparation of Total Saponins in Sanguisorbae Radix

DAI Liang-min; XIONG Yong-ai; YANG Gui-yan; LIN Ying-ying; YANG Ming

doi:10.13422/j.cnki.syfjx.2016180009

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Optimization of Three-step Alkali Precipitation Method for Preparation of Total Saponins in Sanguisorbae Radix

更新时间：2024-01-04

- Optimization of Three-step Alkali Precipitation Method for Preparation of Total Saponins in Sanguisorbae Radix
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 22, Issue 18, Pages: 9-12(2016)
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- DOI：10.13422/j.cnki.syfjx.2016180009
  CLC： R283.6
- Published：2016
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DAI Liang-min, XIONG Yong-ai, YANG Gui-yan, et al. Optimization of Three-step Alkali Precipitation Method for Preparation of Total Saponins in Sanguisorbae Radix[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(18): 9-12.
DOI：

DAI Liang-min, XIONG Yong-ai, YANG Gui-yan, et al. Optimization of Three-step Alkali Precipitation Method for Preparation of Total Saponins in Sanguisorbae Radix[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(18): 9-12. DOI： 10.13422/j.cnki.syfjx.2016180009.

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pH 12～14，静置12 h，离心去沉淀，上清液用10%氢氧化钠溶液调pH 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 extraction and purification technology of total saponins in Sanguisorbae Radix by orthogonal test and three-step precipitation method. Method: HPLC-ELSD method was employed to determine the content of ziyuglycoside-Ⅰ with mobile phase of [methanol-acetonitrile(1:1)]-water for gradient elution.Taking transfer rate of ziyuglycoside-Ⅰ as index

orthogonal test was adopted to optimize extraction technology of total saponins.Three-step alkali precipitation method was used

single factor tests were adopted to optimize purification technology of total saponins with clearance of tannins and ziyuglycoside-Ⅰ content as indexes. Result: The best process was as follows:reflux extracted twice with 8 times the amount of 70% ethanol

each time for 1.5 h

adding 10%NaOH to adjust pH of extract between 12-14

stewing it for 12 hours

collecting supernatant solution after centrifugation

adding 10%NaOH to adjust pH of supernatant solution between 12-13

stewing it for 24 hours

collecting the precipitate after centrifugation

dried the precipitate at 70℃

then reflux extracted 30 min with 30 times the amount of ethanol

vacuum recovery of ethanol

dried 12 h.Purity of total saponins in Sanguisorbae Radix was 91.32%. Conclusion: The optimized extraction and purification technology of total saponins in Sanguisorbae Radix is simple and stable with high yield and purity

which is suitable for industrial production.

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