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Preparation method of lignan in albizia bark

A technology of Albizia Julibrissin and lignans, which is applied to the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems of serious pollution in the operation process, large amount of solvent usage, and low yield, and achieve simple process, The effect of improving product purity and product yield

Active Publication Date: 2019-09-13
南京曼赫医疗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the extraction and separation method of high-purity (-)-syringoresinol-4-O-β-D-apifuranosyl-(1→2)-β-D-glucopyranoside mainly adopts silica gel chromatography Column method, this kind of extraction and separation method has low yield, large amount of solvent usage and serious pollution in the operation process, making it difficult to realize large-scale industrial production

Method used

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  • Preparation method of lignan in albizia bark
  • Preparation method of lignan in albizia bark
  • Preparation method of lignan in albizia bark

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment one: the preparation of a kind of lignan in Albizia julibrissin bark:

[0031] S1: Take 10 kg of Albizia Julibrissin coarse powder, add 60 kg of water, conduct heating and reflux extraction, repeat heating and reflux extraction twice, each time for 1.5 hours, combine the extracts, and filter.

[0032] S2: The filtrate is added to the pretreated HPD-300 macroporous adsorption resin column, the flow rate is controlled at 1BV / h, the effluent is discarded, and 5% ethanol 15000mL is used as the impurity removal agent for impurity removal, and the flow rate is 1BV / h , the eluted impurity removal solution was discarded, and then 20000ml of 50% ethanol solution was used as the eluent for elution, the flow rate was 1BV / h, the collected eluate was concentrated under reduced pressure to syrup, the residue was added with diatomaceous earth, and pulverized into fine powder:.

[0033] S3: Extract 4 times with methanol and dichloromethane mixed solution with a volume ratio...

Embodiment 2

[0035] Embodiment two: the preparation of a kind of lignan in Albizia Julibrissin bark:

[0036] S1: Take 8 kg of Albizia Julibrissin coarse powder, add 120 kg of water, conduct heating and reflux extraction, repeat heating and reflux extraction for 4 times, each time for 1 hour, combine the extracts, and filter.

[0037] S2: The filtrate is added to the pretreated HPD-100 macroporous adsorption resin column, the flow rate is controlled at 2BV / h, the effluent is discarded, and 8000mL of 10% ethanol is used as the impurity removal agent for impurity removal, and the flow rate is 2BV / h , the eluted impurity-removing liquid is discarded, and then eluted with 40% ethanol solution 20000ml as the eluent, the flow rate is 1BV / h, the collected eluate is concentrated under reduced pressure to syrup, the residue is added with diatomaceous earth, and pulverized into fine powder:.

[0038] S3: Extract 5 times with a mixture of methanol and dichloromethane at a volume ratio of 1:7, filter...

Embodiment 3

[0040] Embodiment three: the preparation of a kind of lignan in Albizia julibrissin bark:

[0041] S1: Take 8 kg of Albizia Julibrissin coarse powder, add 80 kg of water, conduct heating and reflux extraction, repeat heating and reflux extraction for 3 times, each time for 3 hours, combine the extracts, and filter.

[0042] S2: The filtrate is added to the pretreated X-5 macroporous adsorption resin column, the flow rate is controlled at 1BV / h, the effluent is discarded, and 12000mL of water is used as the impurity removal agent for impurity removal, the flow rate is 2.5BV / h, wash The removed impurity removal solution was discarded, and then 16000ml of 60% ethanol solution was used as the eluent for elution, the flow rate was 1BV / h, the collected eluate was concentrated under reduced pressure to syrup, the residue was added with diatomaceous earth, and crushed into fine pink:.

[0043] S3: Extract 5 times with methanol and dichloromethane mixture at a volume ratio of 1:8, fil...

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Abstract

The invention provides a preparation method of a lignan in an albizia bark. The method comprises the following steps: s1: grinding albizia bark into coarse powder, carrying out heating relux extraction with a weight ratio of 1:5-15 between albizia bark coarse powder and water, carrying out heating relux extraction for 1-4 times, each time for 1-3 hours, combining the extraction liquid and conducting filtration; s2: adding the filtrate filtered in step s1 to the macroporous adsorption resin column for enrichment, removing impurities with an impurity removal agent, then conducting elution with an eluent, collecting the eluent, conducting concentrating and drying under decompression, and conducting shattering into fine powder; s3: extracting the fine powder prepared in step s2 with extractionsolution for 1-5 times, conducting filtration, combining the filtrates, drying the filtrate and recovering the extraction solution under decompression, and obtaining a residue; and s4: adding methanol to the residue in step s3 for hot dissolution, conducting filtration after dissolution, concentrating the filtrate under decompression to obtain a supersaturated solution, placing the supersaturatedsolution for 2-10 days, conducting crystallizing or recrystallizing, carrying out filtration, collecting solids, and conducting washing and drying. The preparation method is simple in process, and the product yield and product purity are significantly improved.

Description

technical field [0001] The invention relates to a preparation method of a lignan in the bark of Albizia Julibrissin, belonging to the technical field of preparation methods of pharmaceutical preparations. Background technique [0002] Albizia julibrissin bark is the dry bark of Albizia julibrissin Durazz., a leguminous plant, which is stripped in summer and autumn and dried in the sun. It is a commonly used traditional Chinese medicine included in the 2015 edition of "Chinese Pharmacopoeia". The bark of Albizia Julibrissin is sweet in taste and flat in nature, and has the Heart, Liver, and Lung meridians. It has the effects of relieving depression and calming the nerves, promoting blood circulation and reducing swelling. It is often used for restlessness, depression, insomnia, lung abscess, sores, pain from falls, etc. The effective chemical components contained in Albizia Julibrissin are mainly lignans, saponins and so on. Wherein (-)-syringaresinol-4-O-β-D-selfuranosyl...

Claims

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Application Information

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IPC IPC(8): C07H15/26C07H1/08
CPCC07H15/26C07H1/08
Inventor 吴义元梁青
Owner 南京曼赫医疗科技有限公司
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