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Preparation method of rosavin

A technology of ethyl acetate and concentrated liquid, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of low specificity and cumbersomeness of loxavir

Inactive Publication Date: 2012-07-25
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 methods for extracting and preparing roseavid have low specificity and are cumbersome

Method used

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  • Preparation method of rosavin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Take rhodiola rosea raw materials and crush them into 20 meshes, take 1kg, add 10 times the amount of 80% ethanol to extract by cold soaking twice, extract 8 hours each time, combine the extracts to recover ethanol, add appropriate amount of water to dilute, filter, add an equal volume of acetic acid to the filtrate The ethyl ester was fully stirred, the ethyl acetate layer was discarded, the mother liquor was added to the polyamide resin for adsorption, the collection column was concentrated under reduced pressure through the liquid, and 50 g of alumina was added to mix the sample for drying, and then added to a medium-pressure alumina column (diameter-to-height ratio 1:15), Take 10BV of ethyl acetate methanol solution (20:3) for eluting with ethyl acetate methanol, then use ethyl acetate methanol solution (7:3) for HPLC tracking and monitoring, collect high-concentration roseavid fractions, recover reagents, and anhydrous ethanol Dissolve, add diethyl ether dropwise un...

Embodiment 2

[0030] Take rhodiola rosea raw materials and crush them into 60 meshes, take 1kg, add 5 times the amount of 90% ethanol to extract by cold soaking for 3 times, extract for 4 hours each time, combine the extracts to recover ethanol, add appropriate amount of water to dilute, filter, add an equal volume of acetic acid to the filtrate The ethyl ester was fully stirred, the ethyl acetate layer was discarded, the mother liquor was added to the polyamide resin for adsorption, the collection column was concentrated under reduced pressure through the liquid, 80g of alumina was added to mix the sample and dried, and then added to a medium-pressure alumina column (diameter-to-height ratio 1:15), Take 7BV of ethyl acetate methanol solution (4:1) for eluting with ethyl acetate methanol, then use ethyl acetate methanol solution (7:3) for HPLC tracking and monitoring, collect high-concentration rosevin fractions, recover reagents and anhydrous ethanol Dissolve, add diethyl ether dropwise unt...

Embodiment 3

[0032] Take rhodiola rosea raw materials and crush them into 40 meshes, take 1kg, add 8 times the amount of 85% ethanol to extract by cold soaking twice, extract for 10 hours each time, combine the extracts to recover ethanol, add appropriate amount of water to dilute, filter, add an equal volume of acetic acid to the filtrate The ethyl ester was fully stirred, the ethyl acetate layer was discarded, the mother liquor was added to the polyamide resin for adsorption, the collection column was concentrated under reduced pressure through the liquid, and 100g of alumina was added to mix the sample for drying, and then added to a medium-pressure alumina column (diameter-to-height ratio 1:15), Take 8BV of ethyl acetate methanol solution (5:1) for eluting with ethyl acetate methanol solution, then use ethyl acetate methanol solution (7:3) for HPLC tracking and monitoring, collect high-concentration roseavid fractions, recover reagents, and anhydrous ethanol Dissolve, add diethyl ether ...

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Abstract

The invention relates to a preparation method of rosavin, which comprises the following steps: using rose rhodiola as a raw material to break into 20-60 meshes, adding 5-10 times of 80-90% ethanol to perform cold soaking extraction for 2-3 times, recycling the ethanol from the extracted liquid; adding an appropriate amount of water into concentrated liquid to dilute; filtering and adding an equivalent volume of ethyl acetate into the filtrate, agitating sufficiently and abandoning an ethyl acetate layer; adding polyamide resin to adsorb impurities; collecting the liquid passed through the column, depressurizing and concentrating; adding alumina, agitating and drying and then adding into a medium-pressure alumina column, performing gradient elution to the ethyl acetate by methanol, tracing and monitoring by high performance liquid chromatography (HPLC), collecting rosavin flows and recycling reagents; dissolving by anhydrous ethanol and adding an appropriate amount of diethyl ether to refrigerate and crystallize, drying the crystallized matter to obtain pure rosavin. The preparation method provided by the invention adopts the medium-pressure alumina column for separation is short in separation period, large in preparation quantity and suitable for industrial production.

Description

Technical field: [0001] The invention relates to a method for preparing roseavid, in particular to a method for preparing roseavid by using a medium-pressure alumina column. Background technique: [0002] Rosavin is a phenylpropanoid glycoside with molecular formula C 20 h 28 o 10 , molecular weight 428.43, molecular structure [0003] [0004] Physical properties: white transparent needle crystal, melting point 171°C-173°C, soluble in water, ethanol, methanol, butanol, insoluble in ether, chloroform, ethyl acetate. [0005] Roseville is mainly used for anti-fatigue, anti-hypoxia, stress relief, improvement of work efficiency and treatment of functional diseases of the nervous system. [0006] Roseville is mainly derived from the dry roots and rhizomes of Rhodiola rosea, a plant in the Crassulaceae family. [0007] Rhodiola's unique chemical active ingredients are rosavin (the most active), rosin, rosarin, rhodiolin and salidroside. Rhodiola has attracted attention i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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