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Technique for preparing willow leaf tabersonine

A technology of glycyrrhizine and preparation process is applied in the field of preparation of plant extracts, can solve the problems of long production cycle, complex process, low product yield and the like, and achieves short production cycle, simple chemical steps and product yield. high effect

Inactive Publication Date: 2011-05-11
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
  • Technique for preparing willow leaf tabersonine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of preparation technology of willow leaf glycyrrhizin, comprises the following steps successively,

[0018] 1. Raw material pretreatment: African potato fruits are harvested when they are ripe or about to be ripe, dried, crushed, and dried through a 40-mesh sieve for later use;

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

[0020] 3. Purification on the column: select D101 macroporous adsorption resin, directly load the sample with acid water, wash the impurities with water, elute the product with 80% ethanol by mass ratio, and concentrate the eluent under reduced pressure to remove ethanol;

[002...

Embodiment 2

[0023] A kind of preparation technology of willow leaf glycyrrhizin, comprises the following steps successively,

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

[0025] Two, reflux extraction: get 200 grams of seed powder, use 4 times, 3 times, 4 times of mass ratio of volume respectively to be the methanol aqueous solution 60~70 ℃ of 80% reflux extraction three times, be respectively 1 hour, 1.5 hours and 1 hour. Filtrate, combine the filtrates, 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 acid water, wash the impurities with water, elute the product with 90% ethanol water solution by mass ratio, and concentrate the eluent under reduce...

Embodiment 3

[0029] A kind of preparation technology of willow leaf glycyrrhizin, comprises the following steps successively,

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

[0031] Two, reflux extraction: get 200 grams of seed powder, use 3 times, 2.5 times, 2.5 times of mass ratio of volume respectively to be 90% ethanol aqueous solution 70 ℃ of reflux extraction three times, be respectively 1 hour, 50 minutes and 1 hour. Filter, combine the filtrates, concentrate under reduced pressure until there is no alcohol smell, add 500ml of hydrochloric acid aqueous solution with a mass ratio of 0.5%, and set aside;

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

[0033] 4. Alkalini...

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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 preparation of plant extracts, in particular to a preparation process of willow leaf glycyrrhizin. Background technique: [0003] Willow licorice (Tabersonine, CAS NO.4429-63-4) is obtained from oleander plant Amsonia tabemaemontana Walt. (=A.salicifolia) leaves, vinca Cantharanthusroseus (L.) G.Don seeds , Amsonia elliptica Roem.Et Schult. seeds or the seeds of Voacango africana Stapf. 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 ene protons). Glycyrrhizin is currently mainly used to synthesize an anticancer drug: vinpocetine, and it has been proved by animal pharmacological experiments tha...

Claims

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Application Information

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Patent Type & Authority Patents(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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