CN103664669A - Process method for preparing high-purity levodopa - Google Patents
Process method for preparing high-purity levodopa Download PDFInfo
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- CN103664669A CN103664669A CN201210325340.2A CN201210325340A CN103664669A CN 103664669 A CN103664669 A CN 103664669A CN 201210325340 A CN201210325340 A CN 201210325340A CN 103664669 A CN103664669 A CN 103664669A
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- levodopa
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Abstract
The invention discloses a process method for preparing high-purity levodopa. By utilizing chemical characteristics of levodopa, acid water is applied to extract, an impurity removing agent is used for preliminary purifying, and enriching and separating are carried out by virtue of electroosmosis; then, separation is carried out by adopting an isoelectric-point crystallization technology, and a crude crystal is dried to obtain a finished product after being re-crystallized. Process steps are as follows: crushing a mucuna material, adding acid water to extract, adding the impurity removing agent into extracting liquor to remove impurities, filtering, regulating pH value of the liquor to 1-4, entering an electroosmosis device for enriching and separating, regulating the pH value to 3.5, placing at a low temperature of 0 DEG C-4 DEG C, separating out levodopa, regulating acidity of precipitates, adding an antioxidant, placing at the low temperature, separating out crystal, and drying to obtain the finished product. The process method disclosed by the invention adopts the electroosmosis method for enriching and separating the levodopa, so that problems that the levodopa is damaged in an alkaline environment and the like are effectively avoided, and therefore, production period is shortened, energy consumption and cost are lowered; moreover, the method is environmental friendly.
Description
Technical field
The invention belongs to medical technical field, be specifically related to a kind of processing method of preparing high purity levodopa.
Background technology
Levodopa is nonprotein amino acid, and chemical molecular formula is C
9h
11nO
4, molecular weight is 197.19, iso-electric point 3.5,295 ℃ of fusing points.It is a kind of important antiparkinsonian drug, and being used for the treatment of Parkinson's disease etc. has significant curative effect.
Levodopa has three kinds of sources, is respectively chemical synthesis, microbe fermentation method, plant extraction method.According to relevant report, Japanese aginomoto company has Production by Microorganism Fermentation levodopa technology, and America and Europe mainly prepares levodopa by chemical synthesis, and China prepares by plant extraction method.
The problem that plant extraction method mainly exists is that the production cycle is long, and technological process ammoniacal liquor wash-out is big for environment pollution, and global transfer rate is not high, and in production process, energy consumption is larger.
Summary of the invention
The problem existing for solving existing technological process, the object of this invention is to provide a kind of its preparation process that improves the rate of transform, reduces the high purity levodopa of energy consumption and environmental protection.
A kind of processing method of preparing high purity levodopa that the present invention proposes, it is characterized in that, described processing method is to utilize the chemical property of levodopa, with sour water, levodopa is extracted from raw material, first with cleaner, carry out, after preliminary purification, by electrodialysis, levodopa being carried out to enrichment, separation, adopt isoelectric point crystallizing technology to separate out, coarse-grain, after recrystallization, is drying to obtain finished product.Its processing step is:
(1) cat bean material is pulverized, added acidic water extract, extracting liquid filtering;
(2) in extracting solution, add cleaner removal of impurities, filter, obtain solution;
(3) solution regulates pH value 1-4, enters electrodialysis unit and carries out enrichment, separation, and red-tape operati voltage and current, detects discharge port at set intervals, when being no longer the reaction of levodopa, stops electrodialysis, collects feed liquid standby;
(4) feed adjustment pH value to 3.5,0-4 ℃ of low temperature is placed, and filters, and collects precipitate;
(5) precipitate is placed in the pure water that adjusted pH value is 1-3, adds 1% vitamins C, and heating makes to dissolve, add 5% gac, stir 5 minutes, filtered while hot, collects filtrate, 0-4 ℃ of low temperature is placed, crystallization, filters a small amount of absolute ethanol washing of crystallization, in 50 ℃ of following being dried, get product.
In above-mentioned processing method, in step (1), the conditioning agent of sour water is any or two kinds and even multiple mixture in borax, formic acid, acetic acid, lactic acid, boric acid, hydrochloric acid, sulfuric acid, phosphoric acid etc.; In step (2), cleaner is that polymeric flocculant is any or multiple mixture in anionic, cationic, non-ionic type polymeric amide and chitosan; In step (4), pH value conditioning agent is any or two kinds and even multiple mixture in borax, formic acid, acetic acid, lactic acid, boric acid, hydrochloric acid, sulfuric acid, phosphoric acid etc.
Because the present invention has adopted electroosmose process, levodopa is carried out to enrichment, separation, effectively avoided levodopa problem such as destroyed in alkaline environment, shortened the production cycle, reduced energy consumption and cost, and method environmental protection.
Specific embodiments
The present invention first carries out preliminary purification to extracting solution, and extracting solution pH value is controlled in certain scope, by electrodialysis appts enrichment, separated levodopa, and then regulates pH value, makes levodopa at iso-electric point crystallization, and coarse-grain obtains finished product through recrystallization.
Embodiment 1
Take cat beans 1Kg, be broken into coarse particles, add that with formic acid, to be adjusted to PH be 4 sour water, normal temperature dipping extracts 2 times, each 10 times of amounts, after extracting liquid filtering, adding sodium polyacrylate to make its content is 1%, stir, place, filter, filtrate regulates pH value to 3 with hydrochloric acid, carry out electrodialysis, until liquid outlet is no longer levodopa reaction, the pH value of feed liquid is adjusted to 3.5, 0-4 ℃ of low temperature is placed, filter, precipitate is placed in and regulates with hydrochloric acid the pure water that pH value is 1-3, add 1% vitamins C, heating makes to dissolve, add 5% gac, stir 5 minutes, filtered while hot, collect filtrate, 0-4 ℃ of low temperature is placed, crystallization, filter, the a small amount of absolute ethanol washing of crystallization, following dry in 50 ℃, get product.
Embodiment 2
Take cat beans 1Kg, be broken into coarse particles, add that with sulfuric acid, to be adjusted to PH be 3 sour water, decoct and extract 2 times, each 8 times of amounts, after extracting liquid filtering, adding chitosan to make its content is 0.5%, stir, place, filter, filtrate regulates pH value to 3 by boric acid and formic acid mixtures, carry out electrodialysis, until liquid outlet is no longer levodopa reaction, the pH value of feed liquid is adjusted to 3.5, 0-4 ℃ of low temperature is placed, filter, precipitate is placed in and regulates with hydrochloric acid the pure water that pH value is 1-3, add 1% vitamins C, heating makes to dissolve, add 5% gac, stir 5 minutes, filtered while hot, collect filtrate, 0-4 ℃ of low temperature is placed, crystallization, filter, the a small amount of absolute ethanol washing of crystallization, following dry in 50 ℃, get product.
Embodiment 3
Take cat beans 1Kg, be broken into coarse particles, add with hydrochloric acid, it is 2 sour water that the mixing acid that sulfuric acid is made into is adjusted to PH, take diacolation to extract, collect 10 times of amount percolates, adding crosslinking sodium polyacrylate to make its content is 1%, stir, place, filter, filtrate regulates pH value to 3 by boric acid and hydrochloric acid mixture, carry out electrodialysis, until liquid outlet is no longer levodopa reaction, the pH value of feed liquid is adjusted to 3.5, 0-4 ℃ of low temperature is placed, filter, precipitate is placed in and regulates with hydrochloric acid the pure water that pH value is 1-3, add 1% vitamins C, heating makes to dissolve, add 5% gac, stir 5 minutes, filtered while hot, collect filtrate, 0-4 ℃ of low temperature is placed, crystallization, filter, the a small amount of absolute ethanol washing of crystallization, following dry in 50 ℃, get product.
Claims (4)
1. a processing method of preparing high purity levodopa, is characterized in that, take cat beans as raw material, and with acidic water extract, extracting solution, by electrodialytic method, carries out enrichment, separation to levodopa, and concrete operation step is as follows:
(1) preparation of levodopa extracting solution: cat bean material is pulverized, added acidic water extract, extracting liquid filtering;
(2) the preliminary removal of impurities of extracting solution: in the extracting solution making in step (1), add cleaner removal of impurities, filter, obtain the solution of preliminary purification;
(3) enrichment of levodopa, separation: by the solution of step (2) gained, regulate pH value 1-4, enter electrodialysis unit and carry out enrichment, separation, red-tape operati voltage and current, detect at set intervals discharge port, while being extremely no longer the reaction of levodopa, stop electrodialysis, collection feed liquid is standby;
(4), by the feed adjustment pH value to 3.5 of step (3) gained, 0-4 ℃ of low temperature is placed, and filters, and collects precipitate;
(5) by the precipitate of step (4) gained, be placed in the pure water that adjusted pH value is 1-3, add 1% vitamins C, heating makes to dissolve, and adds 5% gac, stirs 5 minutes, filtered while hot, collect filtrate, 0-4 ℃ of low temperature is placed, crystallization, filter, the a small amount of absolute ethanol washing of crystallization, in 50 ℃ of following being dried, gets product.
2. according to a kind of processing method of preparing high purity levodopa claimed in claim 1, it is characterized in that, in described step (1), the conditioning agent of sour water is any or two kinds and even multiple mixture in borax, formic acid, acetic acid, lactic acid, boric acid, hydrochloric acid, sulfuric acid, phosphoric acid etc.; Extracting method is the either type of dipping, decoction, diacolation etc.
3. according to a kind of processing method of preparing high purity levodopa claimed in claim 1, it is characterized in that, in described step (2), cleaner is that polymeric flocculant is any or multiple mixture in anionic, cationic, non-ionic type polymeric amide and chitosan.
4. according to a kind of processing method of preparing high purity levodopa claimed in claim 1, it is characterized in that, in described step (4), pH value conditioning agent is any or two kinds and even multiple mixture in borax, formic acid, acetic acid, lactic acid, boric acid, hydrochloric acid, sulfuric acid, phosphoric acid etc.
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| CN201210325340.2A CN103664669A (en) | 2012-09-05 | 2012-09-05 | Process method for preparing high-purity levodopa |
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| CN201210325340.2A CN103664669A (en) | 2012-09-05 | 2012-09-05 | Process method for preparing high-purity levodopa |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311440A (en) * | 2014-11-05 | 2015-01-28 | 桂林三宝生物科技有限公司 | Method for extracting levodopa from velvet beans |
| CN104402748A (en) * | 2014-12-05 | 2015-03-11 | 南宁知本康业生物技术有限公司 | Microwave-assisted method for extracting levodopa from cat beans |
| CN104610080A (en) * | 2015-01-29 | 2015-05-13 | 黄振忠 | Method for preparing levodopa by using Mucuna pruriens |
| CN107382760A (en) * | 2017-08-18 | 2017-11-24 | 山东鲁抗医药股份有限公司 | A kind of isolation and purification method of levodopa |
| CN108546237A (en) * | 2018-06-15 | 2018-09-18 | 那坡康正天然植物提取有限责任公司 | A method of extracting levodopa by raw material of cat beans |
| CN109081787A (en) * | 2018-09-28 | 2018-12-25 | 那坡康正天然植物提取有限责任公司 | A kind of technique for extracting levodopa from multitude's beans |
| CN109096131A (en) * | 2018-09-28 | 2018-12-28 | 那坡康正天然植物提取有限责任公司 | A kind of technique preparing levodopa using cat beans |
| CN109293521A (en) * | 2018-09-27 | 2019-02-01 | 那坡康正天然植物提取有限责任公司 | A kind of production technology of Chenopodiaceae beans extract |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311440B (en) * | 2014-11-05 | 2016-04-27 | 桂林三宝生物科技有限公司 | A kind of method extracting levodopa from cat beans |
| CN104311440A (en) * | 2014-11-05 | 2015-01-28 | 桂林三宝生物科技有限公司 | Method for extracting levodopa from velvet beans |
| CN104402748A (en) * | 2014-12-05 | 2015-03-11 | 南宁知本康业生物技术有限公司 | Microwave-assisted method for extracting levodopa from cat beans |
| CN104402748B (en) * | 2014-12-05 | 2015-10-21 | 南宁知本康业生物技术有限公司 | A kind of microwave-assisted extracts the method for levodopa from cat beans |
| CN104610080A (en) * | 2015-01-29 | 2015-05-13 | 黄振忠 | Method for preparing levodopa by using Mucuna pruriens |
| CN107382760B (en) * | 2017-08-18 | 2020-04-24 | 山东鲁抗医药股份有限公司 | Separation and purification method of levodopa |
| CN107382760A (en) * | 2017-08-18 | 2017-11-24 | 山东鲁抗医药股份有限公司 | A kind of isolation and purification method of levodopa |
| CN108546237A (en) * | 2018-06-15 | 2018-09-18 | 那坡康正天然植物提取有限责任公司 | A method of extracting levodopa by raw material of cat beans |
| CN109293521A (en) * | 2018-09-27 | 2019-02-01 | 那坡康正天然植物提取有限责任公司 | A kind of production technology of Chenopodiaceae beans extract |
| CN109096131A (en) * | 2018-09-28 | 2018-12-28 | 那坡康正天然植物提取有限责任公司 | A kind of technique preparing levodopa using cat beans |
| CN109081787A (en) * | 2018-09-28 | 2018-12-25 | 那坡康正天然植物提取有限责任公司 | A kind of technique for extracting levodopa from multitude's beans |
| CN109096131B (en) * | 2018-09-28 | 2021-01-15 | 那坡康正天然植物提取有限责任公司 | Process for preparing levodopa by utilizing velvet beans |
| CN109081787B (en) * | 2018-09-28 | 2021-01-15 | 那坡康正天然植物提取有限责任公司 | Process for extracting levodopa from mucuna |
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Application publication date: 20140326 |