CN1305881C - Method for preparing lecithin in high purity - Google Patents
Method for preparing lecithin in high purity Download PDFInfo
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- CN1305881C CN1305881C CNB2004100604578A CN200410060457A CN1305881C CN 1305881 C CN1305881 C CN 1305881C CN B2004100604578 A CNB2004100604578 A CN B2004100604578A CN 200410060457 A CN200410060457 A CN 200410060457A CN 1305881 C CN1305881 C CN 1305881C
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Abstract
The present invention relates to a method for preparing high-purity phosphatidyl choline, which is characterized in that the present invention comprises the following technological processes that plant phosphatide is used as raw material, and low-carbon alcohol and water are used as mixed solvents; then, the plant phosphatide, the low-carbon alcohol and the water are extracted and separated; after a separated alcohol soluble substance is modulated in vacuum by a centrifugal thin film concentrating machine, the alcohol soluble substance enters an aluminium oxide chromatography column so as to carry out chromatographic separation by utilizing a mixed solvent of low-carbon alcohol as an eluting agent; next, the eluting agent after chromatography is concentrated in vacuum and dried so as to obtain a product with the content of phosphatidyl choline as 60 to 95%. Compared with the prior art, the present invention has the advantages that the present invention is capable of producing both phosphatide products with the content of phosphatidyl choline as 35 to 65% and phosphatide products with the content of phosphatidyl choline as 60 to 95%, and the present invention solves the key technical problems of continuous extraction, centrifugal separation, centrifugal thin film concentration, column chromatographic separation and drying, etc. in industrialized production; the present invention can improve the purity, the yield and the quality of phosphatidyl choline products and can reduce production cost, and the present invention has no toxicity and no pollution. The present invention is suitable for large-scale industrialized production.
Description
(1) technical field:
The present invention relates to a kind of preparation method of chemical pharmaceutical prod, particularly be applicable to the preparation method of high-purity phosphatidylcholine of industries such as food, household chemicals, healthcare products and medicine, it is a raw material with plant phosphatide (mainly being soybean phospholipid), the low-carbon (LC) alcohol and water is an extraction agent, adopts Technologies such as continuous extraction, whizzer separation, centrifugal thin-film vacuum concentration, column chromatography purification and vacuum-drying to prepare high-purity phospholipid phatidylcholine product.
(2) technical background
Soybean phospholipid is the product of soybean oil purified byproduct-hydrated oil foot through deep processing, mainly contains one-tenth such as phosphatidylcholine (PC), phosphatidyl cholamine (PE), phosphatidic acid (PA), phosphatidylinositols (PI), sugar ester and glyceryl ester and is grouped into.Phosphatidylcholine is good naturally occurring emulsifying agent and nutrition agent, is widely used in industrial circles such as medicine, food, daily-use chemical industry and healthcare products.Clinically, the high-purity phospholipid phatidylcholine can be used for treating diseases such as atherosclerosis, senile dementia, fatty liver, neurasthenia and malnutrition, and to reducing serum cholesterol, improve blood circulation, preventing cardiovascular disease, and prevent cell aging, brain tonic, reproduction tire curative effect and the health-care effect of rising such as pregnant; Pharmaceutically, also the Chang Zuowei amendment for preparing various pharmaceutical preparations prepares high-fat emulsion and uses, up-to-date studies show that: the high-purity phospholipid phatidylcholine can be used in the transmission and the delivery system of medicament, makes medicine have target, and modern diseases such as inflammation, cancer are directly treated.
Because phosphatidylcholine has good medicines and health protection function and wide application prospect, Chinese scholars is all carried out intensive research to it.At present, the method for the extraction of phosphatidylcholine, separation, purifying is a lot, mainly is raw material with the soybean phospholipid, adopts metal salt precipitate method, CO
2The preparation of technology methods such as supercritical extraction, membrane separation process, column chromatography, solvent-extraction process.The metal salt precipitate method can precipitate in ethanol with the metal complex that metal ion generates phosphatidylcholine according to phosphatidylcholine component in the soybean phospholipid, complex compound non-setting principle in ethanol that other phospholipid fraction and metal ion generate prepares the phosphatidylcholine product, because the dissolving of phosphatide metal complex in ethanol that generates is relative with not dissolving, this method is difficult to produce high-purity phospholipid phatidylcholine product, the phosphatidylcholine metal complex that generates is resolved metal ion process complexity in addition, the operational condition harshness, the inorganic salt that use in the technology can cause environmental pollution; Practical application is few.Openly report CO both at home and abroad
2Phosphatidylcholine product in the supercritical fluid extraction yolk, because overcritical equipment configuration costliness, extraction separation operational condition harshness is difficult to large-scale promotion at present.Membrane separation process is to carry out membrane sepn according to different molecular weight, obtain the phospholipid fraction of different relative molecular weights, therefore isolating key is a separatory membrane, is limited to existing film function close various phospholipid compositions of isolated molecule amount fully still, needs exploitation specific function film ability suitability for industrialized production.Column chromatography is the another kind of method of separation and purification commonly used, key is the selection of stationary phase, eluent, stationary phase sorbent material commonly used has: silica gel, diatomite, silicon-dioxide, aluminium sesquioxide etc., eluent has the mixture of chloroform, normal hexane, sherwood oil, methyl alcohol, low-carbon alcohol or several solvents.Chinese patent publication number CN1429828A patent disclosure to obtain crude lecithin with soybean oil residue after pre-treatment be starting material, be sorbent material with silica gel, carry out column chromatography with methyl alcohol as eluent and separate and obtain high purity lecithin; This method is by crude lecithin purifying high-purity Yelkin TTS, and wash-out adopts refining methanol, easily contaminate environment.Solvent-extraction process is the industrial method of producing the low-purity phosphatidylcholine commonly used, utilizes the different solubility of each phospholipid fraction in solvent, and phosphatidylcholine is separated with other phospholipid fractions.The disclosed method of Chinese patent publication number CN1390843A by powdered soybean phospholipid extraction phosphatidylcholine, the mixed solvent extraction process method of employing acetonitrile and low-carbon alcohol, producing phosphatidylcholine is 70%, yield is 70% product.Owing to adopt the stronger acetonitrile reagent of toxicity to make extraction agent, be difficult to remove acetonitrile solvent in the phosphatidylcholine extract fully, influence the application of phosphatidylcholine product.Therefore, be necessary that exploitation is a raw material with plant phosphatide, avirulent pure water is solvent, take continuous extraction, centrifugation, thin film concentration, chromatographic separation and vacuum drying extraction process, to improving the phosphatidylcholine product purity, yield and quality, and reduce production costs and have great importance.
(3) summary of the invention
Purpose of the present invention is just at existing deficiency in the above-mentioned prior art and the preparation method of a kind of high-purity phospholipid phatidylcholine of special development, it is raw material that this preparation method adopts plant phosphatide, alcohol water is solvent, solved continuous extraction in the suitability for industrialized production, centrifugation, centrifugal thin-film concentrates, chromatographic separation, key issues such as vacuum-drying, can improve the purity of phosphatidylcholine product, yield and quality, reduce production costs, nontoxic pollution-free, be fit to commercial scale production, this Technology both can have been produced the phospholipid prod of phosphatidylcholine content 35-65%, also can produce the product of phosphatidylcholine content 60-95%.
The objective of the invention is to realize by following scheme:
The preparation method of high-purity phospholipid phatidylcholine of the present invention comprises following technological process: with powder plant phosphatide is raw material, low-carbon alcohol and water are mixed solvent, through extracting and separating, isolated pure solvend is after the modulation of centrifugal thin-film thickner vacuum concentration, go into the aluminium sesquioxide chromatography column, mixed solvent with low-carbon alcohol and water is that eluent carries out chromatographic separation, and the elutriant behind the chromatography promptly makes the product of phosphatidylcholine content 60-95% after the vacuum concentration drying.
Among the present invention, the extract after centrifugal thin-film concentrates can directly obtain the product of phosphatidylcholine content 35-65% through vacuum-drying.
Described low-carbon alcohol is any one of ethanol, methyl alcohol, propyl alcohol, the mixed solvent of low-carbon alcohol and water by volume 99.9: 0.1-80: 20, the used centrifugal thin-film thickner vacuum concentration exsiccant vacuum condition of the present invention is 0.09-0.1Mpa, heating condition is 45-80 ℃, concentration time 5-150 minute, the column length of used chromatography column was 1.5 with the diameter ratio: 1-15: 1.
Raw materials used powder plant phosphatide can be powder soybean phospholipid or powder rapeseed oil phospholipid etc.
The raw materials used egg phospholipids that also can be.
Among the present invention, the ratio of powder plant phosphatide and pure water mixed solvent is 1: 0.5-15w/v; The extraction time is 5-180 minute.
The used solid adsorbent of chromatography column is: aluminium sesquioxide or silica gel; The granularity of sorbent material is the 50-500 order.
Eluent behind the chromatography is 0.09-0.10MPa through the dry vacuum tightness of vacuum concentration, and temperature is 40-85 ℃, 30-300 minute concentrate drying time.
Concrete preparation method may further comprise the steps: in a, the mixed solvent stirring extractor with powder soybean phospholipid raw material adding tool low-carbon alcohol and water, stir extraction through a high efficient mixed, make soybean phospholipid fully be distributed in the mixed solvent; B, carry out solid-liquid separation through whizzer, alcohol soluble substance is gone into the extraction liquid storage tank, and alcohol insoluble solids (solid phase phosphatide) carries out reextraction; C, by material: the solvent ratio requirement adds the mixed solvent of low-carbon alcohol and water in the alcohol insoluble solids, carries out the secondary high efficient mixed and stirs extraction; D, extraction fluid are separated with whizzer; E, separation back solid phase phosphatide are gone into the phosphatide storage tank, and pure solvend liquid is gone into the extraction liquid storage tank; F, pure insoluble phosphatide are gone into the vacuum drier drying and are kephalin; Pure solvend in g, the extraction liquid storage tank pumps into the film centrifugal concentrator by solvent pump and carries out vacuum concentration, obtains pure enriched material, and the mixed solvent that evaporates is through condensation, and rectifying is reclaimed, recycled; H, pure enriched material are after modulation jar modulation, and pumping into the aluminium sesquioxide is the chromatography column of sorbent material, are that eluent carries out chromatographic separation with the mixed solvent of low-carbon alcohol and water.Eluent behind i, the chromatography is the product that phosphatidylcholine content is 60-95% through the vacuum decker concentrate drying, and the solvent of evaporation is through condensation, rectifying, recycles.J, pure enriched material are without the chromatography column chromatographic separation, and directly concentrate drying obtains the product that phosphatidylcholine content is 35-65%.
The advantage that the present invention is had compared to existing technology is: this technology can be produced the phospholipid prod of phosphatidylcholine content 35-65%, also can produce the product of phosphatidylcholine content 60-95%; With plant phosphatide is that raw material sources are extensive, and used extraction agent is pure water mixed solvent nontoxicity.Particularly suitability for industrialized production adopts the high efficient mixed extraction, centrifugal continuous separation under the air tight condition, centrifugal thin-film concentrates under the vacuum condition, and chromatographic separation, gordian techniquies such as vacuum-drying, solved the materials abstraction conglomeration, the phosphatide extraction liquid sedimentation bonding that reassembles, alcohol dissolubility material can not be separated preferably with the alcohol insoluble matter material, the oxidation fission of phosphatidylcholine and phospholipid fraction can not be with problems such as polarity size adsorption chromatography separation and purification during concentrate drying, not only make the purity of phosphatidylcholine product, yield and quality improve, and reduced production cost, improved efficiency, production environment is purified, pollution-free, be fit to commercial scale production.
(4) description of drawings
Accompanying drawing is a process flow sheet of the present invention.
(5) embodiment
The present invention is described further in conjunction with specific examples, but does not limit the present invention.
Embodiment 1:
Powder soybean phospholipid raw material 20kg, add low-carbon alcohol water mixed solvent 100L (low-carbon alcohol: water is 90: 10 volume ratios), hybrid extraction 90 minutes after the centrifugation, adds 100L low-carbon alcohol water mixed solvent again in the alcohol insoluble solids, extracted 60 minutes, centrifugation, pure solvend is 70 ℃ in temperature, vacuum tightness be 0.095mPa film centrifugal concentrator concentrate pure enriched material, after the modulation of alcohol enriched material, be that eluent carries out chromatographic separation through aluminium sesquioxide chromatography column, low-carbon alcohol water mixed solvent.Eluent behind the chromatography obtains 4.62kg phosphatidylcholine product through vacuum concentration dry 240 minutes (75 ℃ of temperature, vacuum tightness 0.096Mpa), and high pressure liquid chromatographic analysis is the result show: phosphatidylcholine content is 88.6%, product yield 82.8%.
Embodiment 2:
Powder soybean phospholipid raw material 10kg, add low-carbon alcohol water mixed solvent 20L (low-carbon alcohol: water is 98: 2 volume ratios), 30 ℃ of extraction temperature, hybrid extraction 60 minutes is after the centrifugation, in alcohol insoluble solids, add 30L low-carbon alcohol water mixed solvent again, extracted 60 minutes, centrifugation, pure solvend is 75 ℃ in temperature, vacuum tightness be 0.09MPa film centrifugal concentrator concentrate pure enriched material, pure enriched material separates through aluminium sesquioxide chromatography column chromatography wash-out.Eluent behind the chromatography is 80 ℃ of temperature, and vacuum tightness is under the condition of 0.096MPa, and vacuum concentration obtained 3.05kg phosphatidylcholine product in dry 210 minutes, and high pressure liquid chromatographic analysis is the result show: phosphatidylcholine content is 72.5%, product yield 86.4%.
Embodiment 3:
Powder rapeseed oil phospholipid raw material 10kg, add low-carbon alcohol water mixed solvent 80L (low-carbon alcohol: water is 99: 1 volume ratios), hybrid extraction is 60 minutes under the room temperature, centrifugation adds 20L low-carbon alcohol water mixed solvent again in the alcohol insoluble solids, extracted 45 minutes, centrifugation, the alcohol solvend is 65 ℃ in temperature, vacuum tightness be 0.095MPa film centrifugal concentrator concentrate pure enriched material, pure enriched material is through aluminium sesquioxide chromatography column chromatographic separation.Eluent behind the chromatography, in temperature is 75 ℃, and vacuum tightness is under the condition of 0.098MPa, obtains 2.55kg phosphatidylcholine product in dry 240 minutes through vacuum concentration, high pressure liquid chromatographic analysis is the result show: phosphatidylcholine content is 84.3%, product yield 80.3%.。
Embodiment 4:
Powder soybean phospholipid raw material 10kg, add low-carbon alcohol water mixed solvent 60L (low-carbon alcohol: water is 99: 1 volume ratios), hybrid extraction is 90 minutes under the room temperature, after the centrifugation, the alcohol solvend is 70 ℃ in temperature, vacuum tightness is that vacuum concentration gets pure enriched material in the 0.095mPa film centrifugal concentrator, the alcohol enriched material is 75 ℃ in temperature again, vacuum tightness is under the condition of 0.095MPa, obtained 3.5kg phosphatidylcholine product in 150 minutes through vacuum-drying, high pressure liquid chromatographic analysis is the result show: phosphatidylcholine content is 58.4%, product yield 84.5%.
Embodiment 5:
Concentrating soya lecithin raw material 10kg, add low-carbon alcohol water mixed solvent 30L (low-carbon alcohol: water is 98: 2 volume ratios), 30 ℃ of extraction temperature, hybrid extraction 60 minutes is after the centrifugation, in alcohol insoluble solids, add 20L low-carbon alcohol water mixed solvent again, extracted 30 minutes, centrifugation, pure solvend is 75 ℃ in temperature, vacuum tightness be 0.09mPa film centrifugal concentrator concentrate pure enriched material, pure enriched material separates through aluminium sesquioxide chromatography column chromatography wash-out.Eluent behind the chromatography is 80 ℃ of temperature, and vacuum tightness is under the condition of 0.096mPa, and vacuum concentration obtained 1.45kg phosphatidylcholine product in dry 210 minutes, and high pressure liquid chromatographic analysis is the result show: phosphatidylcholine content is 74.2%, product yield 77.6%.
Claims (8)
1, a kind of preparation method of phosphatidylcholine, it is characterized in that: this preparation method comprises following technological process: with powder plant phosphatide is raw material, low-carbon alcohol and water are mixed solvent, through extracting and separating, isolated pure solvend is after the modulation of centrifugal thin-film thickner vacuum concentration, going into the aluminium sesquioxide chromatography column, is that eluent carries out chromatographic separation with the mixed solvent of low-carbon alcohol and water, and the elutriant behind the chromatography promptly makes the product of phosphatidylcholine content 60-95% after the vacuum concentration drying.
2, the preparation method of phosphatidylcholine according to claim 1 is characterized in that: used low-carbon alcohol is ethanol, methyl alcohol or propyl alcohol; Low-carbon alcohol: the mixed solvent of water by volume 99.9: 0.1-80: 20.
3, the preparation method of phosphatidylcholine according to claim 1 is characterized in that: powder plant phosphatide is powder soybean phospholipid or powder rapeseed oil phospholipid.
4, the preparation method of phosphatidylcholine according to claim 1 is characterized in that: the ratio of powder plant phosphatide and pure water mixed solvent is 1: 0.5-15w/v; The extraction time is 5-180 minute.
5, the preparation method of phosphatidylcholine according to claim 1 is characterized in that: the spissated vacuum condition of centrifugal thin-film thickner vacuum-drying is 0.09-0.1MPa, and heating condition is 45-80 ℃, concentration time 5-150 minute.
6, the preparation method of phosphatidylcholine according to claim 1 is characterized in that: the used solid adsorbent of chromatography column is: aluminium sesquioxide or silica gel; The granularity of sorbent material is the 50-500 order.
7, the preparation method of phosphatidylcholine according to claim 1 is characterized in that: the column length of used chromatography column is 1.5 with the diameter ratio: 1-15: 1.
8, the preparation method of phosphatidylcholine according to claim 1 is characterized in that: the eluent behind the chromatography is 0.09-0.10MPa through the dry vacuum tightness of vacuum concentration, and temperature is 40-85 ℃, 30-300 minute concentrate drying time.
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| CNB2004100604578A CN1305881C (en) | 2004-08-13 | 2004-08-13 | Method for preparing lecithin in high purity |
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| CN1305881C true CN1305881C (en) | 2007-03-21 |
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| CN102633832B (en) * | 2011-02-09 | 2015-07-22 | 北京绿色金可生物技术股份有限公司 | Method for preparing high-purity phosphatidylcholine |
| CN103509047B (en) * | 2012-06-22 | 2016-09-28 | 上海冠硕生物科技有限公司 | The extraction process of the phosphatidylcholine of a kind of antarctic krill and the preparation method of Phosphatidylserine |
| CN102964379B (en) * | 2012-11-16 | 2015-10-21 | 成都圆大生物科技有限公司 | A kind of method preparing phosphatidylserine and phosphatidylcholine |
| CN104230982A (en) * | 2014-10-09 | 2014-12-24 | 陕西源邦生物技术有限公司 | Method for extracting high-content phosphatidylcholine from soybean powder phospholipids |
| CN105037417B (en) * | 2015-07-23 | 2017-04-19 | 沈阳天峰生物制药有限公司 | Method for preparing egg yolk lecithin used for injection through aluminum oxide static adsorption impurity removal and low-temperature sediment oil removal |
| CN107056835A (en) * | 2017-05-12 | 2017-08-18 | 苏州富士莱医药股份有限公司 | A kind of preparation method of lecithin in high purity |
| CN107325125B (en) * | 2017-06-20 | 2019-06-04 | 山东中阳生物科技有限公司 | Soybean oil residue prepare hydrated phospholipids method and its hydrated phospholipids obtained |
| CN110229183B (en) * | 2019-07-25 | 2021-07-20 | (株)斗山 | Production process of egg yolk lecithin |
| CN113201009A (en) * | 2021-04-26 | 2021-08-03 | 南京威尔生物科技有限公司 | Production process of phospholipid for injection |
| CN113173948A (en) * | 2021-04-29 | 2021-07-27 | 南京威尔生物科技有限公司 | A method for preparing various types of natural phospholipids by extraction |
| CN115010750B (en) * | 2022-07-22 | 2023-09-12 | 山东欣康药业有限公司 | Soybean lecithin with high PC (polycarbonate) and PE (polyethylene) ratio and preparation method thereof |
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2004
- 2004-08-13 CN CNB2004100604578A patent/CN1305881C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US2090537A (en) * | 1934-10-27 | 1937-08-17 | Albert A Lund | Lecithin product and process |
| US4235793A (en) * | 1977-04-27 | 1980-11-25 | A. Nattermann & Cie. Gmbh | Process to obtain oily, highly purified phosphatidylcholines |
| US4496486A (en) * | 1980-06-25 | 1985-01-29 | A. Nattermann & Cie. Gmbh | Method for the preparation of phosphatidyl choline of low oil content |
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