CN103467328B

CN103467328B - Method for extracting L-DOPA from velvet beans

Info

Publication number: CN103467328B
Application number: CN201310460648.2A
Authority: CN
Inventors: 蒋元勇; 文继承; 朱昂辉; 易华; 李丽金; 雍小军
Original assignee: GUILIN MINGXING BIOTECHNOLOGY Co Ltd
Current assignee: SANYUAN JINRUI NATURAL INGREDIENTS Co.,Ltd.
Priority date: 2013-09-30
Filing date: 2013-09-30
Publication date: 2014-10-15
Anticipated expiration: 2033-09-30
Also published as: CN103467328A

Abstract

The invention discloses a method for extracting L-DOPA from velvet beans. The method includes the steps that after the velvet beans are crushed, hydrochloric acid with the mass ratio being 1%.-3%. is used for conducting subcritical extraction, after an extracting solution is concentrated, standing, staying overnight and devitrification are carried out, and accordingly a crude extract is obtained; after the crude extract is dissolved by diluted hydrochloric acid, activated carbon is added for conducting reflux, then the activated carbon is filtered and removed, the pH of the filter liquor is adjusted to be 3.0-4.0 by using an alkaline agent, standing, staying overnight and devitrification are carried out, and after drying is completed, a finished product can be obtained. The method for extracting the L-DOPA from the velvet beans is simple in method, few in step, short in time, and a reagent is saved; the yield of the finished product is 2.8%-3.0%, the content can reach up to 98%, a great number of substances such as inorganic salt do not need to be added in the extracting process, exceeding of heavy metal and the like is avoided, and therefore product quality can not be affected.

Description

A kind of method of extracting levodopa from cat beans

Technical field

The present invention relates to the preparation method of a Plant Extracts, specifically a kind of method of extracting levodopa from cat beans.

Background technology

Levodopa (L-DOPA, full name 3,4-dihydroxyphenylalanine) is antiparkinsonian drug, enters cerebral tissue play a role by hemato encephalic barrier, is applicable to primary parkinsonism and non-medicine originality Parkinsonism.The levodopa content of cat beans is up to 5.22%～9.94%.From cat beans, extract at present the existing certain history of natural levodopa.The multiplex sour water alcohol method of traditional extraction technique, levodopa yield is only 1.5% left and right, and the shortcoming of this technique maximum is to evaporate a large amount of extraction agents, and energy consumption is large, and yield is low, and facility investment is many, and cost is high.

Wei Guofeng, Huang Zuliang, He Youcheng etc., reference ion exchange resin method and active carbon adsorption apply to extract the effect in cat beans levodopa, the yield of finding two kinds of methods can reach 2%～3%, but ion-exchange-resin process and active carbon adsorption need the time long, processing material quantity is low, and product purity is lower.

Luo Dongyuan, Wei Xuan, Gong Qin, Wu Sha, the multifarious utmost point etc., membrane process is extracted to cat beans levodopa and study, the levodopa purity of extraction reaches 99.72%, and reusing rate approaches 90%, whole technological process energy consumption is low, pollution less, is not used toxic reagent, has realized cleaner production target.But film used is vulnerable to pollute, and can have influence on product quality; And membrane lifetime is short, need periodic replacement, increased cost.

CN102267919A discloses a kind of preparation method of cat beans levodopa.The method be take cat beans as raw material, take aqueous acid as extracting solvent, after extracting, with water-miscible organic solvent and salts solution and macromolecular water-soluble polymkeric substance, form in proportion double-aqueous phase system, in solution, mean concns reaches 20%～40% partition equilibrium, use again the extraction agent immiscible with two waters to extract, remove respectively impurity, remaining part is by decolouring, crystallization and dry to obtain massfraction be 99.9% levodopa product.But the method step is many, with duration, preparation process adds a large amount of inorganic salt and other material, easily causes the heavy metal etc. of product to exceed standard, and has affected the quality of product.

Summary of the invention

Technical problem to be solved by this invention is to provide a kind of method of extracting levodopa from cat beans, by technique more simple and easy to control, obtains high yield and high-quality cat beans levodopa.

The present invention is by the following technical solutions:

From cat beans, extracting a method for levodopa, is by after the fragmentation of cat beans, with the hydrochloric acid that massfraction is 1 ‰～3 ‰, carries out sub critical extraction, after extracting solution is concentrated, standing, spends the night, and crystallization, obtains crude extract; Crude extract, with after diluted hydrochloric acid dissolution, adds gac to reflux, and then filters and removes gac, with alkaline agent, regulates filtrate pH to 3.0～4.0, standing, spends the night, and crystallization, obtains finished product after being dried.

The hydrochloric acid injection rate of described sub critical extraction is 1～2 times of cat beans weight, and the pressure of extraction is 4.5～5.5MPa, and temperature is 75～85 ℃, and the time is 0.5～1.5h; Preferably, the pressure of described extraction is 5MPa, and temperature is 80 ℃, and the time is 1h.

The add-on of described gac is 0.5 ‰～2 ‰ of the concentrated rear weight of extracting solution, and the time of backflow is 20～60min; Preferably, the add-on of described gac is 1 ‰ of the concentrated rear weight of extracting solution, and return time is 30min.

Described extracting solution is concentrated into 1.5～2.5 times of cat beans weight, is preferably concentrated into 2 times of cat beans weight.

During dissolving, the concentration of dilute hydrochloric acid used is 0.5～1.5mol/L; Preferably, the concentration of this dilute hydrochloric acid is 1mol/L.

Standingly all carry out at ambient temperature for described twice.

Preferably, the massfraction of described hydrochloric acid is 2 ‰.

Preferably, described alkaline agent is ammoniacal liquor.

Preferably, the pH of described filtrate is preferably adjusted to 3.5.

Compared to the prior art, the present invention has the following advantages:

1, the inventive method is simple, and step is few, and the time is short, and leaching process can be saved a large amount of extraction agent; Yield and content are high, and the yield of crude extract is 4% left and right, and content is 75%～80%, and the yield of the finished product is 2.8%～3.0%, and content can reach 98% left and right;

2, the present invention need not add a large amount of inorganic salt and other material, and heavy metal of having avoided product etc. exceeds standard, thereby affects the quality of the finished product.

Embodiment

With embodiment, be further described below, but the present invention is not limited to these embodiment.

Embodiment 1

From cat beans, extract levodopa, step is as follows:

1) will after the fragmentation of cat beans, with hydrochloric acid, carry out sub critical extraction, the massfraction of hydrochloric acid is 2 ‰, injection rate is 1.5 times of cat beans weight, and the pressure of extraction is 5MPa, and temperature is 80 ℃, time is 1h, extracting solution is concentrated into 2 times of cat beans weight, standing under room temperature, spend the night, crystallization, obtains crude extract; The yield of crude extract is 4.1%, and the weight content of levodopa is 80%;

2) crude extract is used after the dissolving with hydrochloric acid of 1mol/L, added extracting solution to concentrate the gac of rear weight 1 ‰, backflow 30min, filters and removes gac, with ammoniacal liquor adjusting filtrate pH to 3.5, standing under room temperature, spends the night, and crystallization, obtains finished product after being dried; The product yield of finished product is 3.0%, and the weight content of levodopa is 98%.

Embodiment 2

From cat beans, extract levodopa, step is as follows:

1) will after the fragmentation of cat beans, with hydrochloric acid, carry out sub critical extraction, the massfraction of hydrochloric acid is 1 ‰, injection rate is 1.5 times of cat beans weight, and the pressure of extraction is 5.5MPa, and temperature is 75 ℃, time is 1h, extracting solution is concentrated into 3 times of cat beans weight, standing under room temperature, spend the night, crystallization, obtains crude extract; The yield of crude extract is 3.9%, and the weight content of levodopa is 78%;

2) crude extract is used after the dissolving with hydrochloric acid of 0.5mol/L, added extracting solution to concentrate the gac of rear weight 1.5 ‰, backflow 60min, filters and removes gac, with ammoniacal liquor adjusting filtrate pH to 3.0, standing under room temperature, spends the night, and crystallization, obtains finished product after being dried; The product yield of finished product is 2.9%, and the weight content of levodopa is 98.2%.

Embodiment 3

From cat beans, extract levodopa, step is as follows:

1) will after the fragmentation of cat beans, with hydrochloric acid, carry out sub critical extraction, the massfraction of hydrochloric acid is 2 ‰, injection rate is 2 times of cat beans weight, and the pressure of extraction is 4.5MPa, and temperature is 80 ℃, time is 1.5h, extracting solution is concentrated into 1 times of cat beans weight, standing under room temperature, spend the night, crystallization, obtains crude extract; The yield of crude extract is 3.8%, and the weight content of levodopa is 79%;

2) crude extract is used after the dissolving with hydrochloric acid of 1mol/L, added extracting solution to concentrate the gac of rear weight 2 ‰, backflow 20min, filters and removes gac, with ammoniacal liquor adjusting filtrate pH to 3.5, standing under room temperature, spends the night, and crystallization, obtains finished product after being dried; The product yield of finished product is 3.0%, and the weight content of levodopa is 97%.

Embodiment 4

From cat beans, extract levodopa, step is as follows:

1) will after the fragmentation of cat beans, with hydrochloric acid, carry out sub critical extraction, the massfraction of hydrochloric acid is 3 ‰, injection rate is 1 times of cat beans weight, and the pressure of extraction is 5MPa, and temperature is 85 ℃, time is 0.5h, extracting solution is concentrated into 2 times of cat beans weight, standing under room temperature, spend the night, crystallization, obtains crude extract; The yield of crude extract is 4%, and the weight content of levodopa is 75%;

2) crude extract is used after the dissolving with hydrochloric acid of 1.5mol/L, added extracting solution to concentrate the gac of rear weight 0.5 ‰, backflow 40min, filters and removes gac, with ammoniacal liquor adjusting filtrate pH to 4.0, standing under room temperature, spends the night, and crystallization, obtains finished product after being dried; The product yield of finished product is 2.8%, and the weight content of levodopa is 97.5%.

Claims

1. from cat beans, extract a method for levodopa, it is characterized in that: by after the fragmentation of cat beans, with the hydrochloric acid that massfraction is 1 ‰～3 ‰, carry out sub critical extraction, after extracting solution is concentrated, standing, spend the night, crystallization, obtains crude extract; Crude extract, with after diluted hydrochloric acid dissolution, adds gac to reflux, and then filters and removes gac, with alkaline agent, regulates filtrate pH to 3.0～4.0, standing, spends the night, and crystallization, obtains finished product after being dried;

The hydrochloric acid injection rate of described sub critical extraction is 1～2 times of cat beans weight, and the pressure of extraction is 4.5～5.5MPa, and temperature is 75～85 ℃, and the time is 0.5～1.5h.

2. method according to claim 1, is characterized in that: the add-on of described gac is 0.5 ‰～2 ‰ of the concentrated rear weight of extracting solution, and the time of backflow is 20～60min.

3. method according to claim 1, is characterized in that: described extracting solution is concentrated into 1.5～2.5 times of cat beans weight.

4. method according to claim 1, is characterized in that: during dissolving, the concentration of dilute hydrochloric acid used is 0.5～1.5mol/L.

5. method according to claim 1, is characterized in that: described alkaline agent is ammoniacal liquor.

6. method according to claim 1, is characterized in that: during sub critical extraction, the massfraction of hydrochloric acid used is 2 ‰.

7. method according to claim 1, is characterized in that: the pressure of described extraction is 5MPa, and temperature is 80 ℃, and the time is 1h.

8. method according to claim 2, is characterized in that: the add-on of described gac is 1 ‰ of the concentrated rear weight of extracting solution, and return time is 30min.

9. method according to claim 1 or 5, is characterized in that: the pH regulator to 3.5 of described filtrate.