CN104311440B - A kind of method extracting levodopa from cat beans - Google Patents
A kind of method extracting levodopa from cat beans Download PDFInfo
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- CN104311440B CN104311440B CN201410619522.XA CN201410619522A CN104311440B CN 104311440 B CN104311440 B CN 104311440B CN 201410619522 A CN201410619522 A CN 201410619522A CN 104311440 B CN104311440 B CN 104311440B
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- levodopa
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- cat beans
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- polyoxyethylene glycol
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Abstract
The invention discloses a kind of method extracting levodopa from cat beans, comprise the steps: Feedstock treating, high pressure extract, aqueous two-phase extraction, desalination, leave standstill, crystallization, obtains levodopa after drying.Have content high, extraction yield is high, and technique is simple, is applicable to producing, the advantages such as production cost is low.
Description
Technical field
The present invention relates to the extracting method of biological technical field, is a kind of method extracting levodopa from cat beans specifically.
Background technology
Cat beans (Mucunacochinchine-sis (Lour) TangetWang.), another name: Li Dou, dragon's paw multitude beans, brave pawl beans, Semen Stizolobii Cochinchinensis, English name: velvetbean.The annual herbaceous species plant of pulse family Mucuna.Stem is cylindrical, climing long 2-10m, multi-branched.Ternately compound leaf, leaflet square round shape is avette.Raceme, papilionaceous corolla, near-white or purple.Originate in Southern Asia and east.China is mainly distributed in the provinces and regions such as south China, southwest and Zhejiang, Jiangxi, Hunan, Guangxi.Happiness warm and moist weather, drought-enduring, barren-resistant, intolerant to waterlogging.Cat beans are a kind of drought-enduring, resistance to thin, farm crop that adaptability is very strong, and root has a lot of root nodule bacterium, and can improve land fertility, root system is more flourishing, and leaf is climing climbs to a higher point, and broad covered area is conducive to conserving water and soil.Cat beans whole body is all precious, and beans shell, beans leaf and beans seed all contain abundant crude fat and crude protein, are superior pig feeds.The levodopa content of cat beans, up to 5.22-9.94%, is the raw material producing levodopa medicine.
Levodopa (L-DOPA, full name 3,4-the second light industry bureau phenylalanine) is antiparkinsonian drug, enters cerebral tissue and plays a role, be applicable to primary parkinsonism and non-medicine originality Parkinsonism by hemato encephalic barrier.
From cat beans, extract natural levodopa has certain history at present.As Chinese patent CN102267919A discloses a kind of preparation method of cat beans levodopa, with cat beans for raw material, take aqueous acid as Extraction solvent, extract rear water-miscible organic solvent and salts solution and macromolecular water-soluble polymkeric substance and form double-aqueous phase system in proportion, in solution, mean concns reaches the partition equilibrium of 20-40%, extract with the extraction agent immiscible with two aqueous phases again, remove impurity respectively, it is 99.9% levodopa product that remaining part obtains massfraction by decolouring, crystallization and drying.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, have impact on the quality of product.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, find that the yield of two kinds of methods can reach 2-3%, but ion-exchange-resin process and active carbon adsorption need the time long, process material quantity is low, and product purity is lower.Luo Dongyuan, Wei Xuan, Gong Qin, Wu Sha, multifarious pole etc., extract cat beans levodopa to membrane process to study, the levodopa purity of extraction reaches 99.72%, and reusing rate is close to 90%, whole technological process energy consumption is low, pollution uses toxic reagent less, not, achieves cleaner production target.But film used is vulnerable to pollute, and can have influence on product quality; And membrane lifetime is short, needs periodic replacement, add cost.The multiplex sour water alcohol method of traditional extraction technique, levodopa yield is only about 1.5%, and the maximum shortcoming of this technique needs 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.
In sum, study a kind of simple possible, the extracting method of easy to operate levodopa has good realistic meaning.
Summary of the invention
The object of this invention is to provide a kind of method extracting levodopa from cat beans, there is technique simple, be applicable to producing, the advantages such as the time is short.
The present invention is achieved through the following technical solutions, and specifically comprises the steps:
1) Feedstock treating: cat beans are broken;
2) high pressure extract: by the raw material after process, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 10-15min, recover normal pressure, filter, obtain extracting solution;
3) be separated: aqueous two-phase extraction is carried out to cat beans, obtain the upper lower phase with extraction mutually of extraction, the double-aqueous phase system that aqueous two-phase extraction uses is made up of polyoxyethylene glycol, sodium hydroxide and water, the mass percent of polyoxyethylene glycol in described double-aqueous phase system is 20-30%, the mass percent of sodium hydroxide in described double-aqueous phase system is 1-5%, surplus is water, and the weight-average molecular weight of described polyoxyethylene glycol is 1000-8000;
4) subsequent disposal: by step 3) phase in the extraction that obtains, desalination, leave standstill, crystallization, obtains levodopa after drying.
Desalination of the present invention preferably adopts ultrafiltration process or dialysis method, and ultrafiltration process employing molecular weight cut-off is the ultra-filtration membrane desalination of 1000-100000, and dialysis method employing molecular weight cut-off is the dialysis tubing desalination of 1000-100000.
Described leaves standstill, and crystallization preferably leaves standstill 12-24h, dwell temperature 0-4 DEG C.
The levodopa that the present invention obtains, detect through HPLC, content is more than 98.5%.
Compared with prior art, advantage of the present invention:
1, prior art is when carrying out the extraction of levodopa, pre-treatment is all generally for solvent with water or ethanol etc., by heating extraction by effective constituent stripping, and the present invention adopts high pressure extract, compare heating to extract, through High Pressure, make the composition such as organic acid, polyphenol, the levodopa energy fully stripping contained in cat beans, be beneficial to the process of subsequent technique, be beneficial to the yield improving activeconstituents.
2, the levodopa content that prior art obtains generally is no more than 98%, the present invention adopts the combination of high pressure extract and aqueous two phase extraction technique, can enhance productivity greatly, prior art column chromatography resin used, for being generally non-polar resin, can only obtain the extract of levodopa content 40-50% through primary sorption; If employing polar resin, also can only obtain levodopa content about 50% through primary sorption, the levodopa wanting to obtain more high-content by 2 times or more Adsorptions, thus must add process time and cost.Aqueous two phase extraction technique is as a kind of novel isolation technique, have mild condition, easy and simple to handle, be easy to series of advantages such as amplifying, separating power is strong, and adopt combine with technique of the present invention, there is the raising of matter, content and the extraction efficiency of levodopa can be increased, compare column chromatography after water extraction or alcohol extracting, the time of the present invention is short, and levodopa content is high.
3, present invention, avoiding the use of a large amount of organic solvent such as dehydrated alcohol, methyl alcohol, environmental protection more.
Embodiment
With embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment 1:
From cat beans, extract a method for levodopa, specifically comprise the steps:
1) Feedstock treating: cat beans are broken;
2) high pressure extract: by the raw material after process, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 10min, recover normal pressure, filter, obtain extracting solution;
3) be separated: aqueous two-phase extraction is carried out to cat beans, obtain the upper lower phase with extraction mutually of extraction, the double-aqueous phase system that aqueous two-phase extraction uses is made up of polyoxyethylene glycol, sodium hydroxide and water, the mass percent of polyoxyethylene glycol in described double-aqueous phase system is 25%, the mass percent of sodium hydroxide in described double-aqueous phase system is 3%, surplus is water, and the weight-average molecular weight of described polyoxyethylene glycol is 1000-8000;
4) subsequent disposal: by step 3) phase in the extraction that obtains, adopt molecular weight cut-off be 1000-100000 ultra-filtration membrane desalination, leave standstill 12-24h, dwell temperature 0-4 DEG C, crystallization, obtains levodopa after drying.
Embodiment 2:
From cat beans, extract a method for levodopa, specifically comprise the steps:
1) Feedstock treating: cat beans are broken;
2) high pressure extract: by the raw material after process, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 15min, recover normal pressure, filter, obtain extracting solution;
3) be separated: aqueous two-phase extraction is carried out to cat beans, obtain the upper lower phase with extraction mutually of extraction, the double-aqueous phase system that aqueous two-phase extraction uses is made up of polyoxyethylene glycol, sodium hydroxide and water, the mass percent of polyoxyethylene glycol in described double-aqueous phase system is 20%, the mass percent of sodium hydroxide in described double-aqueous phase system is 5%, surplus is water, and the weight-average molecular weight of described polyoxyethylene glycol is 1000-8000;
4) subsequent disposal: by step 3) phase in the extraction that obtains, adopt molecular weight cut-off be 1000-100000 dialysis tubing desalination, leave standstill 12-24h, dwell temperature 0-4 DEG C, crystallization, obtains levodopa after drying.
Embodiment 3:
From cat beans, extract a method for levodopa, specifically comprise the steps:
1) Feedstock treating: cat beans are broken;
2) high pressure extract: by the raw material after process, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 12min, recover normal pressure, filter, obtain extracting solution;
3) be separated: aqueous two-phase extraction is carried out to cat beans, obtain the upper lower phase with extraction mutually of extraction, the double-aqueous phase system that aqueous two-phase extraction uses is made up of polyoxyethylene glycol, sodium hydroxide and water, the mass percent of polyoxyethylene glycol in described double-aqueous phase system is 30%, the mass percent of sodium hydroxide in described double-aqueous phase system is 1%, surplus is water, and the weight-average molecular weight of described polyoxyethylene glycol is 1000-8000;
4) subsequent disposal: by step 3) phase in the extraction that obtains, adopt molecular weight cut-off to be the dialysis tubing desalination of 1000-100000, leave standstill 12-24h, dwell temperature 0-4 DEG C, crystallization, obtains levodopa after drying.
Result:
Claims (2)
1. from cat beans, extract a method for levodopa, it is characterized in that:
Comprise the steps:
1) Feedstock treating: cat beans are broken;
2) high pressure extract: by the raw material after process, put into pressure pan, add the pure water of identical weight, be forced into 4kgf/cm
2, make its pressure uniform, and keep 10-15min, recover normal pressure, filter, obtain extracting solution;
3) be separated: aqueous two-phase extraction is carried out to cat beans, obtain the upper lower phase with extraction mutually of extraction, the double-aqueous phase system that aqueous two-phase extraction uses is made up of polyoxyethylene glycol, sodium hydroxide and water, the mass percent of polyoxyethylene glycol in described double-aqueous phase system is 20-30%, the mass percent of sodium hydroxide in described double-aqueous phase system is 1-5%, surplus is water, and the weight-average molecular weight of described polyoxyethylene glycol is 1000-8000;
4) subsequent disposal: by step 3) phase in the extraction that obtains, desalination, leave standstill, crystallization, obtains levodopa after drying.
2. a kind of method extracting levodopa from cat beans according to claim 1, is characterized in that: described leaves standstill, and crystallization, refers to standing 12-24h, dwell temperature 0-4 DEG C.
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| CN201410619522.XA CN104311440B (en) | 2014-11-05 | 2014-11-05 | A kind of method extracting levodopa from cat beans |
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| CN104311440B true CN104311440B (en) | 2016-04-27 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109258928A (en) * | 2017-07-18 | 2019-01-25 | 雷炳忠 | A kind of method of feed is prepared using cat beanpod shell |
| 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 |
| 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 |
| 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3941835A (en) * | 1970-03-19 | 1976-03-02 | Bio-Derivatives Corporation | Recovery of L-Dopa from R-dopa containing materials |
| CN1042703A (en) * | 1988-11-14 | 1990-06-06 | 广西东兰县制药厂 | Water diacolation-ion exchange method is extracted the levodopa novel process |
| 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 |
| CN202124582U (en) * | 2011-07-01 | 2012-01-25 | 安徽普朗膜技术有限公司 | Membrane treatment system capable of extracting levodopa from velvet beans |
| CN103467328A (en) * | 2013-09-30 | 2013-12-25 | 桂林茗兴生物科技有限公司 | Method for extracting L-DOPA from velvet beans |
| CN103664669A (en) * | 2012-09-05 | 2014-03-26 | 李叶华 | Process method for preparing high-purity levodopa |
-
2014
- 2014-11-05 CN CN201410619522.XA patent/CN104311440B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3941835A (en) * | 1970-03-19 | 1976-03-02 | Bio-Derivatives Corporation | Recovery of L-Dopa from R-dopa containing materials |
| CN1042703A (en) * | 1988-11-14 | 1990-06-06 | 广西东兰县制药厂 | Water diacolation-ion exchange method is extracted the levodopa novel process |
| 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 |
| CN202124582U (en) * | 2011-07-01 | 2012-01-25 | 安徽普朗膜技术有限公司 | Membrane treatment system capable of extracting levodopa from velvet beans |
| CN103664669A (en) * | 2012-09-05 | 2014-03-26 | 李叶华 | Process method for preparing high-purity levodopa |
| CN103467328A (en) * | 2013-09-30 | 2013-12-25 | 桂林茗兴生物科技有限公司 | Method for extracting L-DOPA from velvet beans |
Non-Patent Citations (1)
| Title |
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| 左旋多巴提取工艺改进;张晓等;《中国医药工业杂志》;19911231;第22卷(第5期);第207-208页 * |
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