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Method for preparing salidroside from rhodiola rosea

A technology for salidroside and rhodiola, which is applied in the field of process preparation of salidroside, can solve the problems of high aglycone content, short time consumption and high extraction rate, and achieves the effect of improving extraction efficiency and product content

Inactive Publication Date: 2010-07-14
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the patent CN1522746 "a preparation method of Rhodiola medicinal preparation" discloses the method of secondary alcohol precipitation and macroporous resin adsorption, and the content of salidroside is relatively low; "Preparation method of substance", discloses the preparation method of alcohol extraction, organic solvent extraction, purification and separation of D101 macroporous adsorption resin, gradient elution of water and 10%-90% ethanol, etc., the content of salidroside is low, and no separation is obtained. Monomer; Guo Jianpeng et al published "Research on Enzymatic Hydrolysis Process of Rhodiola alpine" in the literature, the enzymatic hydrolysis method is used in the literature, the extraction rate is high, the time is short, but the content of aglycone is relatively high

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  • Method for preparing salidroside from rhodiola rosea

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Effect test

Embodiment 1

[0040] Take the medicinal material Rhodiola rosea, dry and crush it into 20 meshes, take 50kg and add it to an extraction tank filled with 1000L of 70°C water, extract at a constant temperature for 30min, extract 3 times, combine 3000L of extracts, filter, and concentrate to 300L; add 360g of clarifying agent B, Then add 180g clarifier A, centrifuge, take the supernatant, add HPD-100 macroporous adsorption resin, first use 4BV water to elute, then use 20% and 50% ethanol gradient elution successively, the elution speed is 3BV / h , TLC detection; redissolve the salidroside fraction recovery reagent and butanol and pump it into a medium-pressure silica gel column, first remove it with 4BV chloroform, and then elute with chloroform-butanol (7:3), the elution rate is 2BV / h, TLC and HPLC detect at the same time, until there is no salidroside component, collect the fraction containing salidroside, recover the reagent to 1 / 3 of the volume, place crystals, grow crystals, filter out 105...

Embodiment 2

[0042] Take the medicinal material Rhodiola rosea, dry and crush it into 10 meshes, take 10kg and put it into an extraction tank filled with 250L of 80°C water, extract at a constant temperature for 30min, extract twice, combine 500L of extracts, filter, and concentrate to 50L; add 60g of clarifying agent B, Then add 30g clarifier A, centrifuge, take the supernatant, add HPD-100 macroporous adsorption resin, first use 4BV water to elute, then use 20% and 50% ethanol gradient elution successively, the elution speed is 4BV / h , TLC detection; redissolve the salidroside fraction recovery reagent and butanol and pump it into a medium-pressure silica gel column, first elute with 5BV chloroform, then elute with chloroform-butanol (7:3), the elution rate is 1.5 BV / h, TLC and HPLC detection at the same time, until there is no salidroside component, collect the fraction containing salidroside, recover the reagent to 1 / 4 of the volume and place it for crystallization, grow crystals, filte...

Embodiment 3

[0044] Take the medicinal material Rhodiola rosea, dry and crush it into 20 meshes, take 5kg and put it into an extraction tank filled with 80L of 90°C water, extract at a constant temperature for 30min, extract 3 times, combine 240L of extracts, filter, and concentrate to 48L; add 29g of clarifying agent B, Then add 14g clarifier A, centrifuge, take the supernatant, add HPD-100 macroporous adsorption resin, first use 6BV water to elute, then use 20% and 50% ethanol gradient elution successively, the elution speed is 5BV / h , TLC detection; redissolve the salidroside fraction recovery reagent, butanol and pump it into a medium-pressure silica gel column, first eluted with 5BV chloroform, then eluted with chloroform-butanol (7:3), and the elution rate was 2BV / h, TLC and HPLC detect at the same time, until there is no salidroside component, collect the fraction containing salidroside, recover the reagent to 1 / 3 of the volume and place it for crystallization, grow crystals, filter...

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Abstract

The invention relates to a method for preparing salidroside from rhodiola rosea. The process is as follows: taking a rhodiola rosea medicinal material as a raw material, purifying by hot water for 2-3 times, and removing tannin by adding ZTC1+1clarifying agent; centrifuging the obtained liquid supernatant, and adding macroporous absorption resin; carrying out gradient elution by using water and ethanol of different concentrations; separating the separated product by a medium-pressure silicagel column, concentrating an eluent, standing and crystallizing, heating acetone and dissolving coarse grains; and cooling and recrystallizating to obtain the salidroside with high purity. The method has simple production operation and high product purity, and both the macroporous absorption resin and the medium-pressure silicagel column used in the method can be recycled, organic phase used for elution also can be recycled; and the method can expand the industrialization production.

Description

Technical field: [0001] The invention relates to a method for preparing salidroside from Rhodiola rosea, in particular to a method for preparing salidroside through hot water extraction, resin and medium-pressure silica gel column separation and purification. Background technique: [0002] Salidroside, also known as Salidroside, Salidroside. [0003] Molecular formula: C 14 h 20 o 7 [0004] Chemical Name: p-Hydroxyphenylethyl Ethanol Glucopyranoside [0005] Molecular weight: 300.30 [0006] Molecular formula: [0007] [0008] Physical properties: It is colorless transparent needle crystal, melting point 165.5°C-166.5°C, soluble in water, ethanol, methanol, butanol, insoluble in ether, chloroform, ethyl acetate. [0009] The pharmacological activity of Rhodiola is mainly manifested in anti-hypoxia, anti-fatigue, anti-microwave radiation, scavenging free radicals in the body, regulating and restoring the metabolic balance in the human body. Salidroside can restor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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