Method for synchronously separating and preparing salidroside and rosavin from rhodiola rosea

A technology for simultaneous separation of salidroside, applied in chemical instruments and methods, preparation of sugar derivatives, organic chemistry, etc. problem, to achieve the effect of easy to form industrialization, increase utilization value, and simple operation steps

Active Publication Date: 2017-11-03
云南油橄榄大健康产业创新研究发展有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of salidroside (about 6.1%) and rosevin (about 3.6%) in the final product is relatively low, and the separation of salidroside and rosavir has not been realized

Method used

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  • Method for synchronously separating and preparing salidroside and rosavin from rhodiola rosea

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Extraction: 1 kg of Rhodiola root is pulverized, sieved, and the particle size is greater than 60 orders to obtain Rhodiola powder; add 10% ethanol aqueous solution of 8 times the weight of Rhodiola in the obtained Rhodiola powder, which contains low Eutectic solvent (tetraethylammonium chloride: xylitol = 1:1) 9%, reflux extraction, extraction time is 8 hours, continuous extraction 2 times, combined extracts.

[0040] 2) Primary separation and purification: Concentrate the extract to 1 / 4 of the original volume, centrifuge, and pass the supernatant through an expanded bed filled with 0.8 kg of mixed macroporous resin (HPD400A:LSA10:DA201-CIII=1:1.6:3) , Adsorb from bottom to top with a flow rate of 1.5BV / h; after the adsorption is completed, wash from bottom to top with a flow rate of 2BV / h and a dosage of 2.2BV; first elute with 5% ethanol solution from top to bottom Salidroside is produced, the flow rate is 2BV / h, the dosage is 1.5BV, the eluate is collected, conce...

Embodiment 2

[0044] 1) Extraction: 5 kg of rhodiola roots are pulverized, sieved, and the particle size is greater than 60 orders to obtain rhodiola powder; add 50% ethanol aqueous solution of 12 times of rhodiola weight in the obtained rhodiola powder, which contains low Eutectic solvent (tetraethylammonium chloride:glucose=1:2) 5%, reflux extraction, extraction time is 6 hours, continuous extraction 2 times, combined extracts.

[0045] 2) Primary separation and purification: Concentrate the extract to 1 / 4 of the original volume, centrifuge, and pass the supernatant through an expanded bed filled with 5kg of mixed macroporous resin (HPD400A:DA201-CIII=1:5), from bottom to top For adsorption, the flow rate is 2BV / h; after the adsorption is completed, wash from bottom to top, the flow rate of water washing is 3BV / h, and the dosage is 3BV; first use 10% ethanol solution to elute salidroside from top to bottom, the flow rate It is 3BV / h, and the dosage is 2BV. Collect the eluate, concentrate ...

Embodiment 3

[0049] 1) Extraction: 10 kg of rhodiola roots are pulverized, sieved, and the particle size is greater than 60 mesh to obtain rhodiola powder; add 20 times of rhodiola weight 75% ethanol aqueous solution to the obtained rhodiola powder, which contains low Eutectic solvent (tetraethylammonium chloride: xylitol: glucose = 2:1:3) 2%, reflux extraction, extraction time is 4 hours, continuous extraction 2 times, combined extracts.

[0050] 2) primary separation and purification: concentrate the extract to 1 / 4 of the original volume, centrifuge, and pass the supernatant through an expanded bed filled with 8 kg of mixed macroporous resin (HPD400A:LSA10:DA201-CIII=1:1:3), Adsorb from bottom to top with a flow rate of 4BV / h; after the adsorption is completed, wash with water from bottom to top with a flow rate of 4BV / h and a dosage of 4BV; first use 25% ethanol solution to elute the rhododendron from top to bottom Tianside, the flow rate is 4BV / h, the amount of ethanol solution is 3BV,...

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Abstract

The invention discloses a method for synchronously separating and preparing salidroside and rosavin from rhodiola rosea, comprising the following steps: (1) taking the rhodiola rosea as a raw material, and extracting by using analcohol aqueous solution containing a deep-eutectic solvent, wherein the deep-eutectic solvent has the effects of emulsifying, wetting, being assistant in dissolving and the like, and is beneficial for the extraction of the salidroside and the rosavin; (2) preparing a salidrosidecrude extracting solution and a rosavin crude extracting solution respectively from the extract by combining a mixed macroporous resinexpanded bed technology and a gradient elution technology; (3) preparing a salidrosideextract and a rosavin extract from the salidrosidecrude extracting solution and the rosavin crude extracting solution respectively by using the mixed macroporous resinexpanded bed technology again. Through HPLC content testing, the content of the salidroside in the salidroside extract is 40 percent to 80 percent, and the recovery is 60 percent to 88 percent; the content of the rosavin in the rosavinextract is 30 percent to 70 percent, and the recovery is 65 percent to 85 percent.

Description

technical field [0001] The invention relates to the technical field of deep processing of rhodiola medicinal materials, in particular to a method for synchronously separating and preparing salidroside and rosevin from rhodiola. technical background [0002] Rhodiola rosea (Rhodiola rosea L.) is the dry root and rhizome of the perennial herb or subshrub plant of the genus Rhodiola in the family Rhodiola, aliases: Rhodiola rosea, Saul Marble (hidden name), etc., more than 90 species in the world species, distributed in East Asia, Central Asia, Siberia and North America. Rhodiola grows in high-altitude, high-altitude, cold and pollution-free areas, and its growth environment is harsh, so it has strong vitality and special adaptability. It is cold in nature, sweet in taste, astringent, has the effects of promoting blood circulation to stop bleeding, clearing the lungs and relieving cough. It is used to treat pneumonia cough, women's leucorrhea, external use to treat bruises, sc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
CPCC07H1/08C07H15/18
Inventor 刘永峰邸多隆
Owner 云南油橄榄大健康产业创新研究发展有限公司
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