CN103012468A - Method for preparing high-purity egg yolk lecithin through low-temperature solvent precipitation method - Google Patents
Method for preparing high-purity egg yolk lecithin through low-temperature solvent precipitation method Download PDFInfo
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Abstract
The invention relates to a method for preparing high-purity egg yolk lecithin through a low-temperature solvent precipitation method, which comprises the following steps: extracting an egg yolk solution with anhydrous edible alcohol, and then dissolving in short-chain alkane or short-chain alcohol or halogenated hydrocarbon solvent to obtain jelly; dissolving in a cold acetone solution to precipitate out lecithin; and finally washing with cold acetone, and drying to obtain the product. The method is short in extraction process, high in yield and high in product purity (at least more than 90%); and the solvent extraction low-temperature precipitation method is high in treatment capacity, simple in equipment and high in yield.
Description
Technical field
The present invention relates to a kind of poultry egg yolk of utilizing and extract the method for preparing phosphatide, be specifically related to a kind of method of utilizing the low-temperature solvent precipitation technology from egg yolk liquid, to extract egg phospholipids.
Background technology
Phosphatide is prevalent in each tissue of human body and the organ, particularly is present in brain, neural system, heart, lung, kidney, spleen, blood, emulsion, seminal fluid and the sperm, and be biomembranous integral part.Egg phospholipids has very high nutritive value and physiologically active, in Cell protection film, anti-ageing, reducing blood-fat, prevent and treat the aspects such as fatty liver significant curative effect is arranged.Except biological function and medicinal application, phosphatide has in fields such as foodstuffs industry, light industry, chemical industry widely to be used, this is because phosphatide also has the several functions feature, as emulsification, wetting, improve material viscosity, antioxygenation, prevent age of starch etc.
Phosphatide extensively exists in animal and plant body, and is the abundantest with content in the Ovum Gallus Domesticus of fowl egg, account for the 8-10% of dry substance mixture, and Ovum Anas domestica yolk exceeds also more than 0.5 percentage point than egg yolk, so exploitation Ovum Anas domestica yolk Yelkin TTS has more economy.
A lot of researchs have been carried out in the purification of phosphatide both at home and abroad, mainly contain the methods such as solvent extration, supercritical fluid extraction, absorption method, enzyme catalysis method for refining and membrane sepn, wherein front two kinds of methods are mainly used in slightly carrying, obtain PC content and be lower than 70% raw phospholipid, refining purifying obtains PC content and is higher than 70% product and mainly relies on rear three kinds of methods.Solvent extration is traditional PC preparation method.Single solvent is best with the extraction using alcohol effect, and PC extraction yield and content are respectively 71.6% and 51.4%.Mixed solvent extracts best with acetonitrile-methyl alcohol effect, and the extraction yield of PC and content are respectively 67.8% and 72.8%.The soybean oil residue after with an amount of 95% alcohol steep dehydration de-oiling such as Zhang Weinong use ether dissolution behind vacuum concentration, then centrifugation removal solid impurity adds acetone precipitation, obtains PC content and be 65.8% Thick soybeans phosphatide product.The ZnCl such as Hatta
2Ethanol purification of crude phosphatide can be up to 99.6% phosphatide.Complex precipitation with inorganic salts utilizes inorganic salt to the selectivity of phospholipid molecule, although can greatly improve PC content, can introduce in operation metal ion (such as Zn
2+, Cd
2+), affect quality product, add heavily contaminated.Utilize at present the great majority research of organic solvent soaking extraction phosphatide to concentrate on soybean oil residue or the concentrated phosphatide, egg phospholipids is related to less.
LaiBing Sen etc. remove triglyceride level and cholesterol in the yolk powder with the SCF-CO 2 method, use alcohol extraction phosphatide again, obtain the phosphatide total content and be 95% product.Heidlas etc. are take the propane of volume fraction as 70% as entrainment agent, obtain the egg phospholipids total amount and be 85% extract remainder.Lucas Mayer company has announced supercritical CO
2The deoil patented technology of grade lecithin of production, this patented technology not only can adopt continous way or semi continuous technological operation, and the mixing tank operational condition is gentle, can greatly shorten extraction time, extraction agent consumes low, and energy consumption reduces greatly, and production cost also greatly reduces.Supercritical fluid extraction purification phosphatide is a kind of and eco-friendly method, but cost of equipment is relatively more expensive, and can only remove most neutral grease and cholesterol in soybean or the yolk raw material, the strong and dissolving phosphatide ability of molten oily ability a little less than, be only suitable for preparing the raw phospholipid product.
The general sorbent material of selecting of absorption method mainly contains silica gel, and aluminum oxide and ion exchange resin, elutriant are often selected lower alcohol or chloroform equal solvent.Zhang etc. are take soybean oil residue as raw material, and the technique that adopts solvent extration and column chromatography to combine prepares high-purity PC and PE simultaneously, obtain content and be 91.9% PC and a small amount of content and be 74.2% PE product.The lower boiling sherwood oil such as Gunther: C1-4 alcohol: water (1:1:0.175, v/v/v) mixed solvent leaching yolk powder obtains egg phospholipids, and sample introduction is used the mixed solvent wash-out to silicagel column, elutriant is divided into three parts to be collected, and middle portion PC content reaches 94%.Column chromatography equipment is simple, and production cost is low, is present unique method that can be used in the high-purity phosphatide of scale operation, prepares but most of research rests on AG, and the preparation process elutriant reclaims difficult, easily causes environmental pollution.
The people such as Lekh adopt the content of PC in the enzyme process raising phosphatide, the Phospholipid hydrolase of used enzyme source in Caulis et Folium Brassicae capitatae, and its result of study is increased to respectively 95% and 100% with the soybean phospholipid of PC80% and 75% egg phospholipids.But the enzyme process purification can cause cost to increase, and enzyme source is limited, is not suitable for amplifying and produces.
Gupta etc. collect the solution that flows through film with the Thick soybeans phosphatide solution of normal hexane-isopropyl alcohol mixed solvent dissolving by the polypropylene semi-permeable membranes, and evaporation concentration can make PC concentration bring up to 51% by original 25%, and impurity greatly reduces.Membrane sepn is sent out to have that energy consumption is low, device is simple, processing ease, not to produce the new advantages such as pollution, and sepn process is generally carried out at normal temperatures, is particularly suitable for the separating natural material, but film is difficult for regeneration, poor repeatability, and cost is expensive, and industrial being difficult to used.
On this basis, develop a kind of technique simple, cost is low, and equipment requirements is low, and the high-purity phospholipid extraction process that is easy to suitability for industrialized production is very necessary.
Summary of the invention
The objective of the invention is provides a kind of low-temperature solvent precipitator method to prepare the method for high-purity yolk phospholipid for the deficiencies in the prior art.
The concrete technology step is as follows:
1, duck's egg is through cleaning, sterilize, beat eggs, isolate yolk, yolk is through stirring into egg yolk liquid, adding volume is egg yolk liquid volume 3-5 anhydrous edible ethanol doubly, extracted 10min-1 hour 20-40 ℃ of lower the stirring, by filtering to isolate extracting solution, the egg yolk solid that stays repeats to extract twice again, removes egg yolk solid and merges No. 3 extracting solutions, ethanol is removed in 40 ℃ of underpressure distillation, is condensed into jelly;
2, with volume be above-mentioned jelly 1-10 doubly short chain alkanes or the jelly in short chain alcohol or the halogenated alkane dissolution with solvents step 1, filter and remove insolubles, supernatant liquor places-a 20-0 ℃ ice bath is incubated;
Described short chain alkanes can be normal hexane, sherwood oil, Skellysolve A;
Described haloalkane can be hydrocarbon chloroform, methylene dichloride;
Described short chain alcohol can be propyl carbinol, ethanol, methyl alcohol;
3, then slowly pour into volume be supernatant liquor 1-5 doubly-30-0
Cold acetone solution, stirring and evenly mixing, phosphatide Precipitation then, stirring stops, and pours out supernatant liquor;
4, to the phosphatide in the step 3 precipitation with 1-5 times of volume-30-0
Cold acetone washing 5 times, each solvent is removed residual solvent through toppling over removal by cryogenic vacuum oven dry or the nitrogen method of blowing, and obtains the high-purity phospholipid of purity 〉=90%.
The present invention has the following advantages:
1, technique is simple, and is easy to operate, is fit to the heavy industrialization preparation;
2, use convenient solvent reclaiming, the lower and environmental protection of cost;
3, extract flow process short, yield is high, product purity high (purity 〉=more than 90%);
4, solvent extraction low-temperature sludge method treatment capacity is large, and equipment is simple, and productive rate is high;
Table 1 Different Extraction Method relatively
| Extracting method | Phosphatide yield (%) | Phospholipid purity (%) | Characteristics |
| The low-temperature solvent precipitator method | 85-95 | 85-99 | Technique is simple, and phospholipid purity is high, and cost is low, is easy to amplify |
| Conventional solvent-extraction process | 65-80 | 50-90 | Technique is simple, and phospholipid purity is low, and cost is low, is easy to amplify |
| Chromatography column extracts, supercritical extraction | 80-95 | 80-99 | Complex process, phospholipid purity is high, and cost is high, and industrial operation is complicated |
Description of drawings
Fig. 1 is the method process flow sheet that a kind of low-temperature solvent precipitator method of the present invention prepare high-purity yolk phospholipid.
Embodiment
Embodiment 1
The 20g egg yolk liquid places the 100ml triangular flask with magnetic agitation, adds the anhydrous edible ethanol of 60ml, mix and blend 10min.Filter and remove precipitation, supernatant is filled in the round-bottomed flask.The egg yolk solid that stays repeats to extract twice with anhydrous edible ethanol again, removes egg yolk solid, merges No. 3 times extracting solution, and underpressure distillation obtains residual solids after removing ethanol.Residual solids 60ml acetone (4
) the degreasing washing, repeated washing 5 times, product places vacuum drying oven-0.1MPa behind the washing with acetone, and dry 4h under 40 ℃ of conditions obtains the Yelkin TTS crude product, and yield is 76.51%, and phospholipid purity is 89.61%.
Embodiment 2
The 20g egg yolk liquid places the 100ml triangular flask with magnetic agitation, adds the anhydrous edible ethanol of 60ml, mix and blend 30min.Filter and remove precipitation, supernatant is filled in the round-bottomed flask.The egg yolk solid that stays repeats to extract twice with anhydrous edible ethanol again, removes egg yolk solid, merges No. 3 times extracting solution, and underpressure distillation obtains residual solids after removing ethanol.Residual solids places 0 ℃ of ice bath to be incubated with 30ml short chain alkanes (normal hexane, sherwood oil, Skellysolve A) dissolving, then slowly pours 60ml cold acetone (20 into
), stirring and evenly mixing, phosphatide Precipitation then, stirring stops, and supernatant liquor is poured out, and precipitation is with 20ml cold acetone washing 5 times, and solvent is each through toppling over removal.Product places under the room temperature condition nitrogen to blow 12h and removes residual solvent behind the washing with acetone, obtains at last high-purity phospholipid, and total recovery is 91.42%, and phospholipid purity is 95.93%.
Embodiment 3
The 20g egg yolk liquid places the 100ml triangular flask with magnetic agitation, adds the anhydrous edible ethanol of 60ml, mix and blend 60min.Filter and remove precipitation, supernatant is filled in the round-bottomed flask.The egg yolk solid that stays repeats to extract twice with anhydrous edible ethanol again, removes egg yolk solid, merges No. 3 times extracting solution, and underpressure distillation obtains residual solids after removing ethanol.Residual solids places 0 ℃ of ice bath to be incubated with 30ml halogenated alkane (chloroform, methylene dichloride) dissolving, then slowly pours 60ml cold acetone (30 into
), stirring and evenly mixing, phosphatide Precipitation then, stirring stops, and supernatant liquor is poured out, and precipitation is with 20ml cold acetone washing 5 times, and solvent is each through toppling over removal.Product places vacuum drying oven-0.1MPa behind the washing with acetone, and dry 4h under 40 ℃ of conditions obtains high-purity phospholipid at last, and total recovery is 86.13%, and phospholipid purity is 93.28%.
Embodiment 4
The 20g egg yolk liquid places the 100ml triangular flask with magnetic agitation, adds the anhydrous edible ethanol of 60ml, mix and blend 60min.Filter and remove precipitation, supernatant is filled in the round-bottomed flask.The egg yolk solid that stays repeats to extract twice with anhydrous edible ethanol again, removes egg yolk solid, merges No. 3 times extracting solution, and underpressure distillation obtains residual solids after removing ethanol.Residual solids places 0 ℃ of ice bath to be incubated with 30ml short chain alcohol (propyl carbinol, ethanol, methyl alcohol) dissolving, then slowly pours 60ml cold acetone (20 into
), stirring and evenly mixing, phosphatide Precipitation then, stirring stops, and supernatant liquor is poured out, and precipitation is with 20ml cold acetone washing 5 times, and solvent is each through toppling over removal.Product places under the room temperature condition nitrogen to blow 12h and removes residual solvent behind the washing with acetone, obtains at last high-purity phospholipid, and total recovery is 76.54%, and phospholipid purity is 89.73%.
Claims (2)
1. the low-temperature solvent precipitator method prepare the method for high-purity yolk phospholipid, it is characterized in that:
(1) duck's egg is through cleaning, sterilize, beat eggs, isolate yolk, yolk is through stirring into egg yolk liquid, adding volume is egg yolk liquid volume 3-5 anhydrous edible ethanol doubly, extracted 10min-1 hour 20-40 ℃ of lower the stirring, by filtering to isolate extracting solution, the egg yolk solid that stays repeats to extract twice again, removes egg yolk solid and merges No. 3 extracting solutions, ethanol is removed in 40 ℃ of underpressure distillation, is condensed into jelly;
(2) with volume be above-mentioned jelly 1-10 doubly short chain alkanes or the jelly in short chain alcohol or the halogenated alkane dissolution with solvents step 1, filter and remove insolubles, supernatant liquor places-a 20-0 ℃ ice bath is incubated;
(3) then slowly pour into volume be supernatant liquor 1-5 doubly-30-0 ℃ cold acetone solution, stirring and evenly mixing, phosphatide Precipitation then, stirring stops, and pours out supernatant liquor;
(4) to the phosphatide in the step (3) precipitation with 1-5 times of volume-30-0 ℃ cold acetone washing 5 times, each solvent is removed residual solvent through toppling over removal by cryogenic vacuum oven dry or the nitrogen method of blowing, and obtains the high-purity phospholipid of purity 〉=90%.
2. a kind of low-temperature solvent precipitator method according to claim 1 prepare the method for high-purity yolk phospholipid, it is characterized in that:
Described short chain alkanes is normal hexane, sherwood oil or Skellysolve A; Haloalkane is hydrocarbon chloroform or methylene dichloride; Short chain alcohol is propyl carbinol, ethanol or methyl alcohol.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601666A (en) * | 2016-01-12 | 2016-05-25 | 武汉轻工大学 | Method for extracting phospholipid from heads of hypophthalmichthys molitrix and product of method |
| CN107312030A (en) * | 2017-06-12 | 2017-11-03 | 芜湖福民生物药业股份有限公司 | The preparation method of phosphatidyl choline |
| CN111377960A (en) * | 2018-12-28 | 2020-07-07 | 勤亿蛋品科技股份有限公司 | Method for extracting lecithin |
| CN112107687A (en) * | 2019-06-21 | 2020-12-22 | 南京康海磷脂生物技术有限公司 | Method for purifying and separating refined egg yolk powder |
| CN113717221A (en) * | 2021-10-11 | 2021-11-30 | 江苏曼氏生物科技股份有限公司 | Preparation method of high-purity medicinal soybean phospholipid for emulsion |
| CN115043872A (en) * | 2022-06-17 | 2022-09-13 | 哈尔滨工业大学 | Method for extracting deer blood phospholipid and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB412224A (en) * | 1932-12-19 | 1934-06-19 | Hanseatische Muehlenwerke Ag | Improvements in and relating to the production of phosphatide products |
| CN102603790A (en) * | 2012-02-21 | 2012-07-25 | 山东师范大学 | Method for manufacturing high-purity phosphatidylcholine from Antarctic krill |
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2013
- 2013-01-08 CN CN2013100054079A patent/CN103012468A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB412224A (en) * | 1932-12-19 | 1934-06-19 | Hanseatische Muehlenwerke Ag | Improvements in and relating to the production of phosphatide products |
| CN102603790A (en) * | 2012-02-21 | 2012-07-25 | 山东师范大学 | Method for manufacturing high-purity phosphatidylcholine from Antarctic krill |
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| 谢宪章等: "蛋黄中卵磷脂提取方法的研究", 《食品工业科技》, no. 6, 15 December 1997 (1997-12-15), pages 35 - 37 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601666A (en) * | 2016-01-12 | 2016-05-25 | 武汉轻工大学 | Method for extracting phospholipid from heads of hypophthalmichthys molitrix and product of method |
| CN107312030A (en) * | 2017-06-12 | 2017-11-03 | 芜湖福民生物药业股份有限公司 | The preparation method of phosphatidyl choline |
| CN111377960A (en) * | 2018-12-28 | 2020-07-07 | 勤亿蛋品科技股份有限公司 | Method for extracting lecithin |
| CN112107687A (en) * | 2019-06-21 | 2020-12-22 | 南京康海磷脂生物技术有限公司 | Method for purifying and separating refined egg yolk powder |
| CN113717221A (en) * | 2021-10-11 | 2021-11-30 | 江苏曼氏生物科技股份有限公司 | Preparation method of high-purity medicinal soybean phospholipid for emulsion |
| CN115043872A (en) * | 2022-06-17 | 2022-09-13 | 哈尔滨工业大学 | Method for extracting deer blood phospholipid and application thereof |
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Application publication date: 20130403 |