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Method for preparing verbenalin

A technology of verbenaside and ethanol solution, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of high production cost, complicated operation and the like, and achieves low production cost, high purity, and high production technology. simple effect

Inactive Publication Date: 2013-08-07
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such methods are complicated to operate and high in production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Cut the verbena raw material into sections, weigh 10kg, add 10 times the amount of water and heat to 50°C and soak for 2 hours, extract 3 times, combine the extracts and filter with a hollow composite membrane with a molecular weight cut-off of 3000, and then add the permeate to the cut-off Hollow composite membrane nanofiltration with a molecular weight of 200, the concentrated solution is collected and added to a column containing 500g activated carbon resin for adsorption, first eluted with 10 times the column volume of 20% ethanol solution, and then eluted with 8 times the column volume of 80% ethanol solution. The solution was concentrated under reduced pressure until there was no alcohol, added to a column containing 300g alumina resin for adsorption, 8 times the column volume of 90% ethanol solution was eluted, and the eluate was concentrated until the extract was refluxed and dissolved in ethyl acetate solution, filtered and crystallized in cold storage. 9g of...

Embodiment 2

[0019] Cut the verbena raw material into sections, weigh 10kg, add 6 times the amount of water and heat to 60℃ to soak for 2 hours, and extract 3 times. The extracts are combined and filtered with a hollow composite membrane with a molecular weight cut-off of 5000. The permeate is then added to the molecular weight cut-off. 200 hollow composite membrane nanofiltration, collect the concentrated liquid and add it to a 400g activated carbon resin column for adsorption, first eluting with 7 column volume 30% ethanol solution, then 7 column volume 90% ethanol solution, eluent Concentrate under reduced pressure until there is no alcohol, add it to a column containing 400g alumina resin for adsorption, 10 times the column volume of 95% ethanol solution for elution, concentrate the eluate until the extract is refluxed and dissolved in ethyl acetate solution, filtered through refrigeration and crystallized, and dried 9.4 g of white powder was obtained, with a content of 97.7%.

Embodiment 3

[0021] Take the verbena raw material and cut into sections, weigh 10kg, add 7 times the amount of water and heat to 50℃ soak for 2 hours, extract 3 times, combine the extract and filter with a hollow composite membrane with a molecular weight cut-off of 6000, and add the permeate to the cut-off Nanofiltration with a hollow composite membrane with a molecular weight of 200, collect the concentrated solution and add it to a column containing 500g activated carbon resin for adsorption, first eluting with 5 times the column volume of 40% ethanol solution, and then with 6 times the column volume of 90% ethanol solution, eluting The solution was concentrated under reduced pressure until there was no alcohol, added to a column containing 300g alumina resin for adsorption, 8 times the column volume of 95% ethanol solution was eluted, and the eluate was concentrated until the extract was refluxed and dissolved in ethyl acetate solution, filtered and crystallized in cold storage. 10.3...

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Abstract

The invention discloses a method for preparing verbenalin. The method comprises the following steps of: 1) cutting the verbena raw material into segments, adding decuple water for extraction by heating, adding the extract to an ultrafiltration membrane for ultrafiltration, and then adding the filtrate to a nanofiltration membrane for nanofiltration; collecting a concentrated solution, adding the concentrated solution to an activated charcoal column for absorption, performing gradient elution by using an ethanol solution, and performing decompression concentration on elute until no alcohol exists; and 2) adding the concentrated solution to an alumium oxide resin column for absorption, eluting by using the ethanol solution, concentrating the elute, then performing reflux dissolution of the concentrated elute by using the ethyl acetate solution, and finally, crystallizing in cold storage. The method provided by the invention is simple in production process, high in operability, high in purity of the obtained product, and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of biotechnology, in particular to a preparation method of verbenin. Background technique [0002] Verbenoside belongs to iridoid glycosides, CAS No. 548-37-8, molecular formula C 17 h 24 o 10 , molecular weight 388.3, ​​molecular structure formula: [0003] . [0004] Verbena is the whole herb or rooted whole herb of Verbenaceae plant Verbena. It is a perennial herb. The whole herb contains verbenin, tannin, volatile oil and other ingredients. Indications for exogenous fever, damp-heat jaundice, edema and dysentery, diphtheria, amenorrhea, miasma, dental malaria, carbuncle and sores. Verbenain is an iridoid substance in Verbena herb, which has choleretic, purgative and sympathetic inhibitory effects. [0005] Through literature search, the existing methods for preparing verbenin from Verbena generally adopt macroporous resin and silica gel column separation. Such methods are complex in operation and high in...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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