CN1047083A - The separating and purifying method of soy bean mixed phosphatide - Google Patents
The separating and purifying method of soy bean mixed phosphatide Download PDFInfo
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- CN1047083A CN1047083A CN 89103233 CN89103233A CN1047083A CN 1047083 A CN1047083 A CN 1047083A CN 89103233 CN89103233 CN 89103233 CN 89103233 A CN89103233 A CN 89103233A CN 1047083 A CN1047083 A CN 1047083A
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Abstract
A kind of method that can be used as the used for intravenous injection emulsifying agent of from mixing soya beans phosphatide, producing, comprise by main component Yelkin TTS and kephalin in the extracting and separating mixing soya beans phosphatide, respectively kephalin and Yelkin TTS are handled then, the further processing of Yelkin TTS is comprised technologies such as saltouing, dissolve absorption and degreasing.Utilize this method can make oral level and injection stage lecithin emulsifier, also can make oral level kephalin.
Description
The present invention relates to the separating and purifying method of phosphatide, specifically, relate to the method for the soybean phospholipid that from mixing soya beans phosphatide, obtains can be used as the used for intravenous injection emulsifying agent.
The used for intravenous injection emulsifying agent of actual energy industrial-scale production generally has egg phospholipids and soybean phospholipid etc.But the hydrolysis oxidation less stable of egg phospholipids, and China abounds with soybean, and in all kinds of oil crops, contain phosphatide amount the highest (" oil chemistry ", A.A. season Novi Prokofiev work, the Soviet Union) in the soybean, like this, the cost of soybean phospholipid is much lower.Soybean phospholipid except in foodstuffs industry as nutrition agent, emulsifying agent, dispersion agent and stablizer and can be applicable to the aspects such as chemical industry, plastics and military project, it by special extraction, separation means, just be can be used as the emulsifying agent of used for intravenous injection.This used for intravenous injection emulsifying agent is compared with synthetic emulsifying agent etc., has nontoxicity, and good stability can be through advantages such as pressure sterilizings, can be used as the fat milk transfusion of one of the three big key elements of total intravenous nutrition; Be used for preparing liposome with selectivity and immunity; And prepare emulsion as fat-soluble medicine.
The method of purification of phosphatide is generally carried out with conventional method, in U.S. Pat 3798246, has reported soya-bean oil is placed solvent, handles obtaining of light color, edible purifying phospholipid prod with activated silica gel.Among the English Patent BE866461, having reported and used organic solvent, mainly is lower alcohol, and the method for aluminium absorption process purifying phosphatidyl choline.Japanese Patent J53141300 has reported with acetone and lower alcohol elution Yelkin TTS, adds zinc chloride again and handles, and obtains the Yelkin TTS of purifying.
Yet, should remove thermal source preferably as edible phospholipid, just more should be like this when being used for intravenous injection.In prior art and report, or do not have the report of thermal source qualification rate, or the thermal source qualification rate is low, is about 50%.
In addition, according to the separating and purifying method of general mixed phosphatide, raw-material utilization ratio is low, because the kephalin of suitable content is arranged in the mixed phosphatide, and this part kephalin is not utilized, and this wastes very much, especially in plant-scale production.
The object of the present invention is to provide a kind of technology easy, the method for the separation purifying soybean mixed phosphatide that utilization rate of raw materials is high.
It is a kind of when extracting Yelkin TTS from soy bean mixed phosphatide that another object of the present invention is to provide, can also make full use of the method for kephalin, utilize this method to separate after the purifying soybean mixed phosphatide, the Yelkin TTS and the kephalin of oral level can not only be obtained, the Yelkin TTS of injection stage can also be obtained.
The objective of the invention is to finish, soy bean mixed phosphatide use earlier the appropriate solvent extracting and separating, the part that the contains kephalin otherwise processed that leaves aside, the further part that mainly contains Yelkin TTS of having removed kephalin made from extra care based on following design; With saltouing to remove pyrogenic substance; Preferably, the phosphatide after further will saltouing again dissolves processes such as absorption; Degreasing then.
Further describe the separating and purifying method of mixing soya beans phosphatide of the present invention below:
The used raw material of the present invention is a mixing soya beans phosphatide, and its preparation technology comprises toward the crude oil of producing from soybean and adds water, deviates from phosphatide and obtains a mao phosphatide, the concentrated phosphatide that obtains through vacuum hydro-extraction.The used raw material of the present invention is preferably the gained concentrated phosphatide is carried out de-oiling again, and solvent is removed in cryodrying, produces the lower powdery mixing soya beans phosphatide of peroxide value.
Mixing soya beans phosphatide is carried out extracting and separating with appropriate solvent.The main component of mixed phosphatide comprises Yelkin TTS and kephalin, and therefore selected solvent is can these two is isolating, is generally low-grade alkane alcohol, as methyl alcohol, ethanol, propyl alcohol, butanols, wherein is preferably ethanol.This solvent is different to the solvability of the heterogeneity in the phosphatide, and for example, Yelkin TTS is dissolvable in water in the ethanol, and the kephalin difficulty is dissolved in the ethanol.In addition, solvent for use is the pharmaceutical grade specification preferably, like this, just can avoid bringing into the objectionable impurities that does not meet edible or medical requirement in treating processes.Used quantity of solvent is too many, with regard to waste material, and the workload of increase aftertreatment; Very little, just may influence centrifugation, be unfavorable for quality product, and also can increase trouble to aftertreatment.Common consumption is that the weight ratio of the amount of solvent for use amount and mixed phosphatide is 8: 1 to 10: 1, is about 8.5: 1 preferably.Just can obtain the Yelkin TTS that initial gross separation is purified through such processing.Just can be made into oral level soybean lecithin emulsifying agent through concentrating.
Meanwhile, insoluble part is salt-free kephalin, obtains here containing little lower alcohol in the kephalin sediment, helps making milk sap through adding water, and the weight ratio of amount of water and mixed phosphatide is about 3.5: 1, and used water is water recently distilled.Utilize the dry milk sap of spray-drying process just can make the oral level of powdery kephalin.
According to method of the present invention, the first step has just been separated the kephalin that is insoluble to alcohol, makes the purifying process of later Yelkin TTS simplify, and material is saved, and quality further improves, and the suitability for industrialized production ability improves.
Crude lecithin after initial gross separation is purified needs further to handle to be used as the injection stage emulsifying agent, and the removal of heat source substance in the present invention mainly is by the technology of saltouing.After having removed kephalin, remove the thermal source mass treatment thermal source qualification rate is improved greatly.Used salt is preferably anhydrous sodium sulphate; Used water is water recently distilled, and every index meets the injection stage requirement.The amount of handling used salt of saltouing is for just in time making the reach capacity concentration of liquid of treatment solution, and consumption is not only materials waste too much, and can cause the difficulty with aftertreatment; The too little then effect of consumption is bad, saltouts and handles and can carry out several times repeatedly, is preferably 2 to 3 times.
Also contain depressor substance etc. in the crude lecithin, the present invention adopts and to utilize method that appropriate solvent and absorption agent dissolve absorption to remove depressor substance and improve the chromaticness of product and be further purified product.Solvent can be used low-grade alkane alcohol, is preferably ethanol; Absorption agent can be used activated alumina, gac etc.The consumption of activated alumina and mixing soya beans phosphatide is the ratio of the amount of expecting just; Be 0.3: 1 to 0.5: 1 preferably; The consumption of gac is reasonable with the amount of just expecting to be 0.1: 1 to 0.3: 1.Equally, the amount of sorbent material may make adsorption effect descend very little, influences quality product, and consumption is then wasted starting material too much, and may take away phosphatide too much because of adsorption and cause yield to descend.
The present invention further uses acetone treatment to the Yelkin TTS through above-mentioned processing, deoils or fat to remove, and the amount of the consumption of acetone and mixing soya beans phosphatide is in a ratio of about 1: 1.Degreasing can be carried out repeatedly repeatedly, is 2 to 3 times preferably.
Handle mixing soya beans phosphatide according to method of the present invention, can carry out continuously, also can carry out in batches.Easy according to this law technical process, throughput improves, and raw materials consumption reduces, and the mixed phosphatide utilization ratio improves, thereby has improved economic benefit, especially works as method of the present invention and is applied to industrial-scale production, and its effect will be more obvious.
Handle mixing soya beans phosphatide according to method of the present invention, can utilize depleted kephalin in the past, be formed in food, medical science, the useful kephalin product in biological aspect easily.Simultaneously, the technology of preparation Yelkin TTS is improved, and the quality of the Yelkin TTS of oral level and injection stage is improved, and the thermal source qualification rate of product improves, and the step-down qualification rate also obviously improves, and all can reach about 100%.
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
Get 800 gram powdery mixing soya beans phosphatide, toward the heavily steaming ethanol that wherein adds 7000 milliliter 95%, stirring and leaching is 2 hours under 70 ℃ temperature.Then allow its naturally cooling, extract and throw out are separated.And extract placed liquid under 0-5 ℃ temperature, again the clarifying ethanolic soln in upper strata is poured out, be allowed to condition at the nitrogen that feeds through washing, purifying under 70 ℃ of temperature and under the pressure of 750mm Hg, carry out underpressure distillation, obtain sticking jelly, be crude lecithin.
Embodiment 2
Add the water recently distilled that 4800 milliliters of every indexs all meet the water quality requirement of injecting specification in the crude lecithin of the evaporate to dryness that in embodiment 1, obtains, under 80 ℃ of temperature, stir and make its dissolving, add 750 gram anhydrous sodium sulphate then while stirring, then be warming up to about 100 ℃, about 10 minutes, remove liquid.Add 2000 milliliters of water recently distilleds again, under 80 ℃ temperature, stir and make its dissolving, add 350 gram anhydrous sodium sulphate then, be warming up to about 100 ℃, about 10 minutes, remove liquid, get the precipitating thing.With the temperature of in 70 to 75 ℃ of this precipitating things, the following drying of pressure of 750mm Hg, obtain sticking jelly.
Embodiment 3
The heavily steaming ethanol that adds 7000 milliliter 95% in embodiment 2 in the viscose glue shape Yelkin TTS of gained stirs the mixture and it was placed liquid under 0 to 5 ℃ temperature, filters then.In filtrate, add 240 gram activated aluminas, stirred this mixture 1 hour down, filter then in 40 ℃.In this filtrate, add 176 grams, 767 type gacs, stirred 1 hour, filter then.Then in nitrogen purge gas atmosphere, under 70 ℃, the condition of 750mm Hg, gained filtrate is carried out underpressure distillation, obtain sticking jelly.
Embodiment 4
In the sublimed sticking jelly of embodiment 3 gained, add an amount of anhydrous propanone, grind repeatedly and embathe, so repeat 3 to 4 times, till acetone solution is clarification.Dry under 40 ℃, the condition of 750mm Hg again, obtain sticking jelly, be refined lecithin.
To products therefrom and repeatedly repeat above-mentioned experiment products therefrom and carry out a series of quality index analysis: recording nitrogen content with Kjeldahl determination is 1.6 to 2.1%; Recording phosphorus content with the molybdenum blue colorimetric method is 3.5 to 4.3%; Use potentiometry, recording pH in 1.2% phospholipid aqueous solution is 5.5 to 9.0; Record iodine value 90 to 110 with the Webster method; Recording acid value by Chinese Pharmacopoeia version in 1963 is＜12, peroxide value＜75 milligramequivalents/kilogram sample.
Carry out heat source check by Chinese Pharmacopoeia version in 1963,3% concentration, the rabbit test dose is 10 ml/kg.Carry out the step-down inspection by Chinese Pharmacopoeia version in 1963,3% concentration, reduced pressure experiment dosage is 1 ml/kg.
Embodiment 5
Safety inspection
Getting 10 heavily is the small white mouse of 18 to 20 grams, to 1 milliliter of every execution tail vein injection, observes 5 to 7 days, does not all have destruction.The toxicity test result of small white mouse is:
LD mg/kg=6686 ± 641
Embodiment 6
The water recently distilled of throw out among the embodiment 1 with 2800 milliliters mixed, and heated and stirred becomes milk sap, is spray dried to the powdery product then.
Claims (22)
1, a kind of separating and purifying method that mainly contains the soy bean mixed phosphatide of Yelkin TTS and kephalin is characterized in that this method comprises:
(a) the soy bean mixed phosphatide extracting and separating is become Yelkin TTS and kephalin crude product;
(b) Yelkin TTS of saltouing and obtaining by (a).
2, in accordance with the method for claim 1, it is characterized in that extracting used solvent is the low-grade alkane alcohol that is selected from methyl alcohol, ethanol, propyl alcohol and butanols etc.
3, in accordance with the method for claim 2, it is characterized in that described low-grade alkane alcohol is an ethanol.
4, according to claim 2,3 described methods, the weight ratio that it is characterized in that the material quantity of quantity of solvent and soy bean mixed phosphatide is 8: 1 to 10: 1.
5, in accordance with the method for claim 4, the weight ratio that it is characterized in that the material quantity of quantity of solvent and soy bean mixed phosphatide is 8.7: 1.
6,, it is characterized in that extraction liquid with gained further places under 0 to 10 ℃ the environment according to claim 2,3 described methods.
7, in accordance with the method for claim 1, the used salt that it is characterized in that saltouing is anhydrous sodium sulphate.
8, in accordance with the method for claim 3, the used salt that it is characterized in that saltouing is anhydrous sodium sulphate.
9,, it is characterized in that saltouing and handle and to carry out more than 1 time or 1 time according to claim 7,8 described methods.
10, in accordance with the method for claim 1, it is characterized in that this method comprises that also the product to (b) gained dissolves adsorption treatment.
11, in accordance with the method for claim 10, it is characterized in that dissolving adsorption process is to be selected from one group of low-grade alkane alcohol that comprises methyl alcohol, ethanol, propyl alcohol and butanols.
12, in accordance with the method for claim 10, it is characterized in that described adsorption treatment is that absorption agent carries out with the activated alumina.
13, in accordance with the method for claim 10, it is characterized in that described adsorption treatment is that absorption agent carries out with the gac.
14, in accordance with the method for claim 10, it is characterized in that described adsorption treatment can be to use activated carbon treatment again with activated alumina earlier.
15, in accordance with the method for claim 14, the consumption that it is characterized in that activated alumina and gac was respectively 0.2: 1 to 0.5: 1 and 0.1: 1 to 0.3: 1 with the material quantity ratio of soy bean mixed phosphatide.
16, in accordance with the method for claim 8, it is characterized in that using gac again with activated alumina earlier, is that solvent dissolves adsorption treatment with ethanol.
17, in accordance with the method for claim 1, it is characterized in that this method also comprises carries out degreasing to (b) products therefrom.
18, in accordance with the method for claim 17, it is characterized in that skimming treatment can carry out more than 1 time or 1 time.
19, in accordance with the method for claim 17, it is characterized in that with acetone being that solvent carries out skimming treatment.
20, in accordance with the method for claim 10, it is characterized in that this method also comprises further carries out skimming treatment.
21, in accordance with the method for claim 1, it is characterized in that the kephalin sediment after the extraction is mixed with water, heated and stirred is made milk sap, again spraying drying.
22, in accordance with the method for claim 20, the weight ratio that it is characterized in that the material quantity of amount of water and soy bean mixed phosphatide is 3.5: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89103233 CN1047083A (en) | 1989-05-10 | 1989-05-10 | The separating and purifying method of soy bean mixed phosphatide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 89103233 CN1047083A (en) | 1989-05-10 | 1989-05-10 | The separating and purifying method of soy bean mixed phosphatide |
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| CN1047083A true CN1047083A (en) | 1990-11-21 |
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| CN 89103233 Pending CN1047083A (en) | 1989-05-10 | 1989-05-10 | The separating and purifying method of soy bean mixed phosphatide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224514A (en) * | 2013-05-07 | 2013-07-31 | 上海艾韦特医药科技有限公司 | Production technology of high-purity egg yolk lecithin |
| CN104981167A (en) * | 2012-12-20 | 2015-10-14 | 卡吉尔公司 | Method for the purification of lecithin |
| CN108066768A (en) * | 2017-11-17 | 2018-05-25 | 江苏曼氏生物科技股份有限公司 | A kind of preparation process of high purity medical soybean lecithin |
| CN108552476A (en) * | 2018-04-16 | 2018-09-21 | 广东日可威富硒食品有限公司 | A kind of Fermented Noodles with Tomato Nutrients and preparation method thereof |
-
1989
- 1989-05-10 CN CN 89103233 patent/CN1047083A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104981167A (en) * | 2012-12-20 | 2015-10-14 | 卡吉尔公司 | Method for the purification of lecithin |
| CN103224514A (en) * | 2013-05-07 | 2013-07-31 | 上海艾韦特医药科技有限公司 | Production technology of high-purity egg yolk lecithin |
| CN108066768A (en) * | 2017-11-17 | 2018-05-25 | 江苏曼氏生物科技股份有限公司 | A kind of preparation process of high purity medical soybean lecithin |
| CN108552476A (en) * | 2018-04-16 | 2018-09-21 | 广东日可威富硒食品有限公司 | A kind of Fermented Noodles with Tomato Nutrients and preparation method thereof |
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