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Preparation method of high-purity reinioside C

A technology of lotus chrysanthemum and lotus saponin, which is applied to the preparation of sugar derivatives, chemical instruments and methods, steroids, etc., can solve the problems of large solvent capacity, small preparation amount, complicated operation, etc., and achieve less reagent consumption , continuous preparation, large amount of preparation

Inactive Publication Date: 2013-02-06
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As mentioned above, the existing method adopts the separation of silica gel column, the solvent capacity is large, the sample loss is serious, and the operation is complicated, while the gel column is separated from the preparation liquid phase, the cycle is long, and the preparation volume is small.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Pulverize the medicinal material of chrysanthemum chrysanthemum, take 2kg, add 10 times of 90% methanol for ultrasonic extraction twice, each time for 1 hour, add 150g of diatomaceous earth to the extract recovery reagent, dry it, pack it into a column, wash it with acetone until there is no flavonoid component, and then The saponin was eluted with 400ml of 50% methanol solution, and the collected eluent was concentrated under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water, and mix them in a separatory funnel according to 3:1:4. After fully layering, take the lower phase and fill the high-speed countercurrent chromatography spiral tube, turn the host, adjust the speed to 700rpm, and pump The upper phase is used as the mobile phase. After dynamic equilibrium, the flow rate is adjusted to 2ml / min. The extract is dissolved in the mobile phase, and the sample is injected through the injection valve. The components are collected according to th...

Embodiment 2

[0014] Pulverize the medicinal material of the lotus chrysanthemum, take 2kg, add 6 times 80% methanol and ultrasonically extract 3 times, each time for 1 hour, add 150g of diatomaceous earth to the extract recovery reagent, dry it, pack it into a column, wash it with acetone until there is no flavonoid component, and then The saponins were eluted with 600ml of 30% methanol solution, and the collected eluate was concentrated under reduced pressure to obtain an extract. Take ethyl acetate, n-butanol and water, and mix them in a separatory funnel according to 7:3:6. After fully layering, take the lower phase and fill the high-speed countercurrent chromatography spiral tube, turn the host, adjust the speed to 900rpm, and pump The upper phase is used as the mobile phase. After the dynamic equilibrium, the flow rate is adjusted to 2ml / min. At the same time, the extract is dissolved with the mobile phase, and the sample is injected through the injection valve. The components are coll...

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PUM

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Abstract

The invention discloses a preparation method of high-purity reinioside C. The method comprises the steps that: a polygala aureocauda Dunn medicine material is crushed; 6-10 time amount of 80-90% methanol is added, and the mixture is subjected to ultrasonic extraction 2-3 times; a reagent of the extraction liquid is recovered; diatomite is added to the extraction liquid, and the mixture is dried; the mixture is loaded on a column; acetone is used for washing until no flavonoid content is left; a 30-50% methanol solution is used for eluting saponin; an obtained material is concentrated and is subjected to high-speed countercurrent chromatography separation; a component is collected according to a spectrum; and the component is vacuum-dried, such that the high-purity reinioside C is obtained. When the method is adopted for preparing reinioside C, the efficiency is high, a period is short, a yield is high, and product purity is no lower than 98%.

Description

technical field [0001] The present invention relates to a preparation method of high-purity chrysanthemum saponin C, in particular to a method for preparing high-purity chrysanthemum saponin C by high-speed countercurrent chromatography. Background technique [0002] Reinioside C (reinioside C) is a triterpenoid saponin, amorphous white powder, no obvious melting point, molecular formula C 63 h 98 o 31 , molecular weight 1350, soluble in water, methanol, n-butanol, insoluble in petroleum ether, ether, benzene. [0003] Polygala aureocauda Dunn is the root or whole plant of Polygala aureocauda Dunn, a plant of the genus Polygala in the family Polygala. According to traditional medicine, it tastes sweet, slightly bitter, flat, and has the effects of nourishing qi and blood, invigorating the spleen and removing dampness, promoting blood circulation and regulating menstruation. Treatment of uterine prolapse, leucorrhea, and irregular menstruation. Modern studies have shown ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司