Preparation method of high-purity salidroside

A salidroside and high-purity technology, applied in the field of preparation of high-purity salidroside, can solve the problems of organic solvent residue, high energy consumption, low separation efficiency, etc., to improve purity and yield, and improve resource utilization rate, the effect of ensuring the separation effect

Active Publication Date: 2016-02-03
四川天晟制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method uses multi-step solvent extraction combined with silica gel column and polyamide column chromatography, which has the disadvantages of wasting organic solvent, high energy consumption, low separation efficiency, residual organic solvent and high labor intensity
Although high-speed countercurrent chromatography (HSCCC) can be used to prepare high-purity salidroside, this method also has the disadvantages of high cost, residual organic solvents and unsuitability for industrialization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Pretreatment: Take the decoction pieces of Rhodiola angustifolia, crush them into coarse powder; refer to the percolation method of liquid infusion and extract, use 95% ethanol (mass fraction) equal to the weight of the coarse powder, stir and soak for 1 hour;

[0025] Rough extraction: add 65% ethanol solution to the soaked coarse powder, so that the coarse powder is completely immersed in the ethanol solution, soak for 24 hours and then infiltrate, collect the leachate and concentrate it in a vacuum at low temperature, recover the solvent ethanol, and the concentrated solution is the leachate.

[0026] Macroporous resin purification: absorb the supernatant of the leachate after standing still, and use weakly polar AB-8 macroporous resin to adsorb and remove polysaccharides and proteins. The specific steps for removing polysaccharides and proteins are as follows: after loading the supernatant, wash it with purified water until it is colorless, the volume of purified wat...

Embodiment 2

[0030] Pretreatment: Take the decoction pieces of Rhodiola angustifolia, crush them into coarse powder; refer to the percolation method of liquid infusion and extract, use 95% ethanol (mass fraction) equal to the weight of the coarse powder, stir and soak for 1 hour;

[0031] Rough extraction: add 65% ethanol solution to the soaked coarse powder, so that the coarse powder is completely immersed in the ethanol solution, soak for 24 hours and then infiltrate, collect the leachate and concentrate it in a vacuum at low temperature, recover the solvent ethanol, and the concentrated solution is the leachate.

[0032] Macroporous resin purification: absorb the supernatant of the leachate after standing still, and use weakly polar AB-8 macroporous resin to adsorb and remove polysaccharides and proteins. The specific steps for removing polysaccharides and proteins are as follows: after loading the supernatant, wash it with purified water until it is colorless, the volume of purified wat...

Embodiment 3

[0037] Pretreatment: Take the decoction pieces of Rhodiola angustifolia, crush them into coarse powder; refer to the percolation method of liquid infusion and extract, use 95% ethanol (mass fraction) equal to the weight of the coarse powder, stir and soak for 1 hour;

[0038] Rough extraction: add 65% ethanol solution to the soaked coarse powder, so that the coarse powder is completely immersed in the ethanol solution, soak for 24 hours and then infiltrate, collect the leachate and concentrate it in a vacuum at low temperature, recover the solvent ethanol, and the concentrated solution is the leachate.

[0039] Macroporous resin purification: absorb the supernatant of the leachate after standing still, and use weakly polar AB-8 macroporous resin to adsorb and remove polysaccharides and proteins. The specific steps for removing polysaccharides and proteins are as follows: after loading the supernatant, wash it with purified water until it is colorless, the volume of purified water...

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PUM

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Abstract

The invention discloses a preparation method of high-purity salidroside, which comprises the following steps: crushing rhodiola sachalinensis as a raw material, and then adding a 95% ethanol solution for soaking and percolating; sucking supernatant liquid after the percolate is in a standing state, and adsorbing by using weak-polar macroporous resin to remove polysaccharide and protein; sampling, then washing with purified water until the supernatant liquid is colorless, and carrying out gradient elution; separating a salidroside crude product in a RP-HPLC (Reversed-Phase High Performance Liquid Chromatography), and carrying out gradient elution by taking a methanol aqueous solution as a mobile phase; when the target peak occurs, collecting elution solutions in sections; and freeze-drying the elution solution in which the purity of salidroside is higher than 98%, thereby obtaining high-purity salidroside. According to the invention, impurities including saccharide and protein are removed by percolation and macroporous resin adsorption to obtain the salidroside crude product; after the impurities including saccharide and protein are removed, the degree of purification of the RP-HPLC can be favorably improved; and through reasonable gradient elution and elution solutions, the purity and yield of the product are further increased.

Description

technical field [0001] The invention relates to the technical field of methods for extracting effective components of traditional Chinese medicines, in particular to a method for preparing high-purity salidroside. Background technique [0002] Rhodiola is a perennial herbaceous plant or subshrub wild plant belonging to the Sedum family Rhodiola. It has rich plant resources and many varieties. There are about 96 species in the world and 73 species in my country. Salidroside in Rhodiola is the unique active ingredient of this plant, which has the functions of strengthening the body, reconciling yin and yang, nourishing and strengthening the body, etc. Modern pharmacological studies have proved that salidroside has preventive and anti-dementia effects, anti-deficiency Oxygen effect, anti-aging effect and inhibition of rapid ventricular arrhythmia, clinically used to treat coronary heart disease, high altitude hypotension, high altitude polycythemia. Toxicity test showed that t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 刘霞谭杨杨罗芯茹谢婷婷
Owner 四川天晟制药有限公司
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