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Two-step resin method for preparing salidrose

A technology of salidroside and rhodiola can be used in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., and can solve the problems of small preparation amount, inability to large-scale production, long separation process time, etc. simple craftsmanship

Inactive Publication Date: 2010-11-03
常州朗诣节能技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses many kinds of separation media, dextran gel is expensive, and silica gel cannot be recycled. The whole separation process takes a long time and costs high, which is not suitable for industrial production.
The preparation of salidroside by high-speed countercurrent liquid chromatography has produced a gram-grade product at present, and the product obtained has high purity. The disadvantage is that the preparation amount is small, and the high-speed countercurrent liquid chromatography equipment is expensive and cannot be produced on a large scale.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Take 500 grams of Rhodiola rosea crude extract, add 5000 ml of water to dissolve, heat to 30 ° C, stir and keep warm for 2.5 hours. Filtration gave a clear filtrate. The filtrate was adjusted to pH 3, and flowed through the column of HZ-816 adsorption resin (Shanghai Huazhen Science and Technology Co., Ltd.) at normal temperature, and then passed through 1200ml of 30% ethanol to collect the effluent. Concentrate the effluent to syrup, add HZ-816 adsorption resin, mix evenly and dry. According to the ratio of dried adsorbent resin: packed adsorbent resin = 1:6, add the dried resin to the chromatographic column filled with HZ-816 adsorbent resin, and pass through 15% ethanol solution at normal temperature for chromatography. The chromatographic solution was collected and concentrated to dryness. Add ethanol to dissolve, heat to 50°C, and filter while hot. Concentrate the filtrate, cool to 0°C, crystallize out, and recover the filtrate for mechanical use. After the sa...

Embodiment 2

[0012] Take 500 grams of Rhodiola rosea crude extract, add 5000 ml of water to dissolve, heat to 70 ° C, stir and keep warm for 1 hour. Filtration gave a clear filtrate. The filtrate was adjusted to pH 4, and flowed through the column of Amberlite XAD-4 adsorption resin (product of RohmHaas Company, USA) at normal temperature, and then 2000 ml of 25% ethanol was passed through to collect the effluent. After the effluent was concentrated to syrup, Amberlite XAD-4 adsorption resin was added, mixed evenly and dried. According to the ratio of dried adsorbent resin: packed adsorbent resin = 1:2, add the dried resin to the chromatographic column filled with Amberlite XAD-1600 adsorbent resin (product of RohmHass, USA), and pass it under normal temperature. 20% ethanol solution was used for chromatography, and the liquid was collected and concentrated to dryness. Add n-butanol to dissolve, heat to 50°C, and filter while hot. Concentrate the filtrate, cool to 0°C, crystallize out, ...

Embodiment 3

[0014] Take 500 grams of Rhodiola rosea crude extract, add 5000 ml of water to dissolve, heat to 60 ° C, stir and keep warm for 1.5 hours. Filtration gave a clear filtrate. The filtrate was adjusted to pH 3, and flowed through the column of HZ-816 adsorption resin (Shanghai Huazhen Technology Co., Ltd.) at room temperature, and then 2500 ml of 15% methanol was passed through to collect the effluent. After the effluent is concentrated to a syrupy state, add HZ-816 adsorption resin, mix evenly and dry. According to the ratio of the dried adsorption resin: the adsorbed resin that has been packed = 1:10, the dried resin is added to the chromatographic column that has been filled with HZ-816 adsorbed resin, and 5% methanol solution is passed into it at normal temperature. Chromatography, the liquid was collected and concentrated to dryness. Add n-butanol to dissolve, heat to 50°C, and filter while hot. Concentrate the filtrate, cool to 0°C, crystallize out, and recover the filtr...

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Abstract

This invention relates to a method for separating and preparing high-purity rhodiola root glycosides from natural rhodiola root crude extract using two-step resin method, comprising: dissolve the rhodiola root crude extract in the 20-90Def C water with stirring followed by filtration, adjust the filtrate pH to 1-5 then load on the absorption resin column at room temperature, elute with organic solvent like acetone, low-carbon alcohol or acetate, concentrate the eluent, and load on the chromatography column at room temperature, concentrate and evaporate the chromatography liquid to dryness, then add in organic solvent like low-carbon alcohol or acetate and heat to re-dissolve, filtrate and concentrate the filtrate to precipitate the crystals, then obtain the high-purity rhodiola root glycosides after filtration. By using one resin absorption and one resin chromatography, this invention can prepare high-purity rhodiola root glycosides with 90%-98% purity from low-content(1%-5%) natural rhodiola root crude extract, and the absorption and chromatography process is done at room temperature. Besides, the process is easy and qualified for industrial production.

Description

technical field [0001] The invention relates to a method for separating and preparing salidroside (salidroside) from crude extracts of natural plants Rhodiola rosea, belonging to the technical field of biochemical industry. Background technique [0002] The sedum family Rhodiola is a perennial herb or subshrub plant. There are more than 90 species in the world, and nearly 80 species in China. Most of them grow on limestone, granite mountains, and valley rocks at an altitude of 3,500 to 5,000 meters. Rhodiola resources in my country are mainly distributed in some areas in the northeast, northwest, north and southwest of China. Studies have shown that Rhodiola has biomedical effects such as anti-hypoxia, anti-fatigue, anti-aging, anti-radiation, anti-tumor, lowering blood fat and preventing cardiovascular diseases. Salidroside is the main active ingredient in Rhodiola rosea. [0003] It is reported in the literature that the preparation of salidroside is mostly completed by ...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/08
Inventor 陈骏徐环昕刘坐镇周晓明江邦和
Owner 常州朗诣节能技术有限公司
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