Technique for preparing willow leaf tabersonine

A willow-leaf glycyrrhizin and preparation technology, applied in the field of preparation of plant extracts, can solve the problems of long production cycle, low product yield, complicated process, etc., and achieve short production cycle, high product yield, chemical steps simple effect

Inactive Publication Date: 2008-08-27
XIAN HAO TIAN BIO ENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a preparation process of glycyrrhizin to overcome the problems of complex process, long production cycle and low product yield in the prior art

Method used

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  • Technique for preparing willow leaf tabersonine
  • Technique for preparing willow leaf tabersonine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A preparation process of willow glycyrrhizine includes the following steps in sequence:

[0018] 1. Raw material pretreatment: The African horse bell fruit is harvested when it is ripe or about to mature, dried, crushed, and dried through a 40-mesh sieve for use;

[0019] 2. Reflux extraction: Take 200 grams of seed powder and extract with 4 times, 3 times, and 3 times the volume of n-hexane at 50°C for three times with 1 hour each time. Filter, combine the filtrate, wash the n-hexane layer three times with 750 ml of a 1% hydrochloric acid aqueous solution by mass, recover the organic solvent, and combine the acid aqueous solution for use;

[0020] 3. Purification on the column: D101 macroporous adsorption resin is selected, the acid water solution is directly loaded, the impurities are washed with water, the product is eluted with ethanol with a mass ratio of 80%, and the eluate is concentrated under reduced pressure to remove the ethanol;

[0021] 4. Alkalization and extr...

Embodiment 2

[0023] A preparation process of willow glycyrrhizine includes the following steps in sequence:

[0024] 1. Raw material pretreatment: African horse bell fruit is harvested when it is ripe or about to mature, dried, crushed, and dried through a 50-mesh sieve for use;

[0025] 2. Reflux extraction: Take 200 grams of seed powder and extract with 4 times, 3 times, and 4 times volume of 80% methanol aqueous solution at 60-70°C under reflux for three times, respectively, for 1 hour, 1.5 hours and 1 hour. Filter, combine the filtrate, concentrate under reduced pressure until there is no alcohol, add 500ml of hydrochloric acid aqueous solution with a mass ratio of 1.5%, and set aside;

[0026] 3. Purification on the column: choose XDA-6 macroporous adsorption resin, directly load the sample with the acid water solution, wash the impurities with water, elute the product with a 90% ethanol aqueous solution by mass, and concentrate the eluate under reduced pressure to remove the ethanol;

[...

Embodiment 3

[0029] A preparation process of willow glycyrrhizine includes the following steps in sequence:

[0030] 1. Raw material pretreatment: African horse bell fruit is harvested when it is ripe or about to mature, dried, crushed, and dried through a 50-mesh sieve for use;

[0031] 2. Reflux extraction: Take 200 grams of seed powder and extract with 3 times, 2.5 times, and 2.5 times volume of 90% ethanol aqueous solution at 70°C for three times, respectively, for 1 hour, 50 minutes and 1 hour. Filter, combine the filtrate, concentrate under reduced pressure until there is no alcohol taste, add 500ml of 0.5% hydrochloric acid aqueous solution by mass, and set aside;

[0032] 3. Purification on the column: use XDA-7 macroporous adsorption resin, directly load the sample with acid water solution, wash impurities with water, elute the product with 60% ethanol, and concentrate the eluate to remove the ethanol;

[0033] 4. Alkalization and extraction: add 200ml of water to the concentrated sol...

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Abstract

The invention relates to a preparation method of plant extract, in particular to a preparation method of willow leaf tabersonine, which can resolve the problems of prior art such as complex process, long production period and low product yield. The preparation method comprises 1, material pretreatment: breaking and drying seeds, 2, heating, refluxing, extracting and acidifying, 3, purifying on column, 4, alkalizing, extracting, washing hexane layer via water and removing solvent to obtain the product. The preparation method has the advantages of simple chemical process, low environment pollution, high safety, short production period, support for large-scale industrial production, simple process, high controllability and high product yield, wherein unit kilogram of Africa potato can produce at least 98% willow leaf tabersonine whose yield is higher than 1.6%.

Description

[0001] Field: [0002] The invention relates to the technical field of the preparation of plant extracts, and in particular to a preparation process of glycyrrhizinine. Background technique: [0003] Tabersonine (Tabersonine, CAS NO. 4429-63-4) is derived from the oleander plant Amsonia tabemaemontana Walt. (=A. salicifolia) leaves, Catharanthus roseus (L.) G. Don seeds , Oval leaf water Licorice Amsonia elliptica Roem.Et Schult. Seeds or the African wakanga tree Voacango africana Stapf seeds. Its chemical name is Aspidospermidine-3-carboxylic acid, 2,3,6,7-tetradehydro-(5α,12β,19α)-methylseter, and its molecular formula is C 21 H 24 N 2 O 2 , The molecular weight is 336.42. Its physical state is oily liquid, and its hydrochloride (ethanol) melting point is 199~199.5℃, [α] D 25 -333°(C=2.5, methanol), 13 C-NMR: δ 5.75 (2H, sharp peak, two alkene protons). Willow glycyrrhizin is currently mainly used to synthesize an anti-cancer drug: Vinpocetine, and it has been confirmed by anima...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/16A61P35/00A61K36/24
Inventor 张小燕詹彦李艳宋晚平徐小琴
Owner XIAN HAO TIAN BIO ENG TECH
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