CN1028225C - New process for extracting levodopa by use of water percolation-ion exchange method - Google Patents
New process for extracting levodopa by use of water percolation-ion exchange method Download PDFInfo
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- CN1028225C CN1028225C CN 88107959 CN88107959A CN1028225C CN 1028225 C CN1028225 C CN 1028225C CN 88107959 CN88107959 CN 88107959 CN 88107959 A CN88107959 A CN 88107959A CN 1028225 C CN1028225 C CN 1028225C
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- levodopa
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Abstract
The present invention relates to a novel technology for extracting levodopa from cat beans in mucuna plant seeds. The present invention is characterized in that a diluted acid solution with strong permeability is used as the solvent, levodopa is extracted at room temperature by using the percolation method, the exchange is carried out through 732<#> cation exchange resin, and a mixed liquor with ammonia water and acetic acid glacial is used as an eluting agent so as to purify and extract the levodopa. Compared with the alcohol extraction technique, the present invention enhances the yield by more than twice with obvious economic benefit.
Description
The invention belongs to plant extract amino acids material, particularly the cat beans extract the novel process of levodopa medicine.
Levodopa is to treat Parkinson's disease medicine preferably at present.Levodopa can be by chemical synthesis process production, also can extract from lamb's-quarters bean plant seed such as lamb's-quarters beans, broad bean, cat beans.
According to reported in literature, 1971 and American scholar Bell in 1972 and Daxenbichler are from lamb's-quarters bean plant seed, with hot water extraction, anionite-exchange resin AG1 * 2 absorption, 10% Glacial acetic acid is that the research of eluent extraction separation levodopa is achieved success, yield is 3.1～6.7%(1046J, AGR, FOOD, CHEM, VOL20, NO, 5,1972).
Daxenbichler extracts levodopa with hot water-ion exchange method, and raw material is lamb's-quarters bean plant seed (Mucuna Seed), and lab scale feeds intake and is that 100g, yield are 3.1～6.7%.This technological advantage is to use hot water extraction, and solvent can get, and purifies, separates the yield height with Zeo-karb (AG1 * 2); With 10% Glacial acetic acid is eluent, and consumption is few, is beneficial to concentratedly, and cost is low, but this Process heat water yield is difficult for greatly filtering, and increases exchange capacity, is unfavorable for big production.The used anionite-exchange resin of this technology (AG1 * 2) is domestic does not simultaneously produce, and Daxenbichler technology can't be used for domestic production.
The objective of the invention is to seek and utilize home-made starting material, chemical reagent (eluent) to extract the levodopa novel process,, improve the quality, reduce cost, increase economic efficiency to improve yield with the diverse ion exchange method of Daxenbichler technology.
The object of the present invention is achieved like this: the cat bean powder is broken into 18～60 order meal, is solvent with 0.1%～0.25% aqueous hydrochloric acid, extracts with the diacolation method, and extracting solution is by 732
#Storng-acid cation exchange resin exchange (or extracting solution solidifies protein denaturation and separates out earlier by being heated to 100 ℃, and after the filtering protein impurities, clear filtrate is again by 732
#The Zeo-karb exchange), again with washing the impurity such as protein that are adsorbed on the resin in the The suitable solvent hydrochloric acid soln, be 4～7 with 1% ammonia soln and with Glacial acetic acid accent pH at last, as the levodopa eluent levodopa wash-out is gone out, elutriant is through concentrating, cooling crystallization, refining and levodopa.Its technical process is as follows:
Cat beans (pulverizing)/(18-60 order) cat beans meal (0.1%～0.25% aqueous hydrochloric acid)/(immersion was oozed 36 hours) percolate (filtration, Zeo-karb exchange, eccysis protein, wash-out)/((or be heated to 100 ℃ earlier, filtrate is passed through resin again)) washing lotion (concentrating)/(600mmHg) concentrated solution (0 ℃ of-10 ℃ of cooling)/(crystallization filters) crude product (making with extra care)/() levodopa.
This process using diacolation method is extracted, the Ex-all method of protein, and select for use suitable resin to claim eluent, make the levodopa in the cat beans extract more complete; Resin has more firm adsorption to levodopa, the protein impurities that is adsorbed on the resin is not easily washed out levodopa by the eccysis of protein eluent, the levodopa eluent can fully wash out levodopa, thereby reach purification, isolating best effect, thereby reach purification, isolating best effect, and can improve the quality, improve yield, increase economic efficiency.
Technology of the present invention has following characteristics:
1. used diluted acid solvent has stronger perviousness, and strength of solution all is in the gradient state in the diacolation process, utilizes levodopa stripping, diffusion, so the solvent of usefulness is few, extracts more fully, and extracting solution reaches more than 85%.
2. used resin is a storng-acid cation exchange resin, domestic production, and can guarantee produce to need, and this resin selective adsorption levodopa preferably, and levodopa and other impurity are separated.Used eluent can more fully come out the levodopa wash-out that is adsorbed on the resin, and levodopa is purified, good separating effect, and quality product is high and stable, and yield can reach 3.34%.
3. eluent is easy to get inexpensively, and consumption few (lacking about 1/2 than extracting solution) reduce to concentrate amount and energy-conservation significantly, is beneficial to reduce cost, and economic benefit is very remarkable.
4. equipment requirements is not high, and is easy and simple to handle understandable.
Embodiment:
Take by weighing qualified cat beans 5000 grams, be ground into 18-60 order meal, evenly be sprinkled in the extracting cylinder of the 30L0.12% aqueous hydrochloric acid for preparing earlier, soaked under the room temperature 2～4 hours, diacolation 36 hours is according to a conventional method then measured percolate levodopa content when few, stop diacolation, collect percolate 100L altogether, filtering, clear filtrate is by 732
#Storng-acid cation exchange resin (plastic resin treatment according to a conventional method) exchange, flow 10L～12L per hour, exchange finishes, with 0.6% left and right sides hydrochloric acid soln 50L flushing resin, remove deproteinize, behind the Ex-all protein, extremely neutral with the deionized water rinsing resin, transfer about pH6.5 with Glacial acetic acid with 1% ammonia soln then, solution is the eluent wash-out, collect elutriant 30L altogether, under the 600mmHg vacuum, contract deeply, have mass crystallization to separate out to 1500ml with the glass film thickener, 10 ℃ were cooled off 8 hours in refrigerator, inclining supernatant liquor (reclaiming levodopa with the liquid reconcentration), and suction filtration washs to washing lotion with pure water and to clarify, drain, weigh wet crude product 302 grams, by thick wet product amount preparation 1mol hydrochloric acid (analytical pure) liquid 1170ml, the suitable oxidation inhibitor that adds, pour crude product into and constantly be stirred to dissolving fully, add 9 gram gacs, stirred 5 minutes, with the B suction filtration that is covered with an amount of charcoal layer, get the about 1480ml of clear filtrate, under constantly stirring, slowly add 3.5mol ammoniacal liquor and transfer pH4.0, have mass crystallization to separate out, put in the refrigerator and cooled off 8 hours under 10 ℃, just go out supernatant liquor (concentrating the recovery levodopa) with liquid, suction filtration with pure water washing 3 times, is drained, dewater with dehydrated alcohol 50ml, drain elaboration 210 grams that to wet, 60 ℃ of oven dry, get elaboration 152 grams, reclaim to such an extent that levodopa elaboration 15 restrains altogether with liquid, be total to such an extent that elaboration 167 restrains, yield is 3.34%.Elaboration is by " Chinese pharmacopoeia 85 years version checks, conformance with standard fully.
Claims (2)
1, a kind of method of extracting levodopa with water diacolation-ion exchange method from the cat beans, it is characterized in that with 0.1～0.25% hydrochloric acid soln be solvent, exchanging by 732 type storng-acid cation exchange resins, is eluent with 0.5～2% ammoniacal liquor, and transferring pH with Glacial acetic acid is 4-7.
2, technology according to claim 1 is characterized in that isolating protein solvent-concentration of hydrochloric acid solution is 0.5-0.7%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88107959 CN1028225C (en) | 1988-11-14 | 1988-11-14 | New process for extracting levodopa by use of water percolation-ion exchange method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88107959 CN1028225C (en) | 1988-11-14 | 1988-11-14 | New process for extracting levodopa by use of water percolation-ion exchange method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1042703A CN1042703A (en) | 1990-06-06 |
| CN1028225C true CN1028225C (en) | 1995-04-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88107959 Expired - Fee Related CN1028225C (en) | 1988-11-14 | 1988-11-14 | New process for extracting levodopa by use of water percolation-ion exchange method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1028225C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109232288A (en) * | 2018-09-27 | 2019-01-18 | 那坡康正天然植物提取有限责任公司 | A kind of method of Chenopodiaceae beans production levodopa |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267919A (en) * | 2011-05-31 | 2011-12-07 | 南宁市一锋生物科技有限公司 | Preparation method of L-dopa from Mucuna pruriens |
| CN103664669A (en) * | 2012-09-05 | 2014-03-26 | 李叶华 | Process method for preparing high-purity levodopa |
| 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 |
| CN105372367B (en) * | 2015-11-10 | 2017-06-06 | 苏州大学 | A kind of detection method of lamb's-quarters beans extract |
| 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 |
-
1988
- 1988-11-14 CN CN 88107959 patent/CN1028225C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232288A (en) * | 2018-09-27 | 2019-01-18 | 那坡康正天然植物提取有限责任公司 | A kind of method of Chenopodiaceae beans production levodopa |
| CN109232288B (en) * | 2018-09-27 | 2021-11-23 | 那坡康正天然植物提取有限责任公司 | Method for producing levodopa by using chenopodium quinoa |
| 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 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1042703A (en) | 1990-06-06 |
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