CN1179426A - Refining process for high-purity yolk phospholipid - Google Patents
Refining process for high-purity yolk phospholipid Download PDFInfo
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Abstract
A process for refining high-purity yolk phospholipid includes such technological steps as loading yolk as raw material in extractor, passing supercritical CO2 into the extractor, removing triglyceride and cholesterol under supercritical condition, introducing supercritical CO2 gas containing alcohol into said extractor, and separating out yolk phospholipid under supercritical condition, and features simple apparatus, easy operation, high purity and recovery rate of product and resulting in three kinds of products.
Description
The present invention relates to the preparation method of high-purity phospholipid, more precisely the preparation method of high-purity egg phospholipids.
Phosphatide is the lipid of the phosphorous acid group of a class, is histiocytic ultimate constituent, has important biological function.Containing highly unsaturated fatty acids in the phosphatide, is the important source of human body polyenoic acid.It has cholesterol (Ch) and triglyceride level (TG) content that reduces in the blood, improves lipid metabolism and arteriosclerotic function.Phospholipid molecule is the soluble molecule of typically holding concurrently, and has emulsification function preferably, is the ultimate constituent of liposome, is again the important component of total intravenous nutrition emulsion.It has higher medical value, brain tonic, beauty treatment, anti-ageing, reducing blood-fat is arranged, protect the liver effect such as enrich blood, and has a wide range of applications in each fields such as chemical industry, light industry, foodstuffs industry.
Yolk contains phosphatide and reaches 18% at most in animal, the plant, and soybean is 1.82%, and the former is 9.9 times of the latter, and the main raw material that extracts phosphatide is soybean (extraction soybean phospholipid) and yolk (egg phospholipids).Topmost composition is Yelkin TTS (PC) in the phosphatide, contains PC 72.6% in the egg phospholipids, contains PC 16～21% in the soybean phospholipid.
The phosphatide of needed by human body is mainly from natural foods such as yolk and soybean, but along with science and technology development and growth in the living standard, phosphatide is reduced, and body increases the demand of phosphatide, thereby easily cause the phospholipid nutritive relative deficiency, so phosphatide is unrestricted foodstuff additive in the developed country.Along with improving constantly of China's living standards of the people, the demand of phosphatide is increasing.
The method of extracting phosphatide from whole food has two kinds: a kind of is chemical extraction method, and second kind is the physical extraction method.
Said chemical extraction method is exactly to utilize ethanol, ether, chloroform, acetone and other organic solvent to extract the method for extracting phosphatide repeatedly.Though chemical extraction method can obtain the phosphatide of higher degree, but step is various, process is tediously long, makes phosphatide easy oxidized hydrolysis in extraction process, and its stability reduces, thereby causes the downgrade of phosphatide.In addition, chemical extraction method will add more chemical reagent, comprising a large amount of organic solvents.Because phosphatide is used in medicine, food and the makeup more, so must be removed, but still there is the quality of micro-organic solvent influence phosphatide.Moreover with the egg phospholipids of chemical extraction method preparation, wherein content of cholesterol is still higher, promptly uses acetone treatment, and the content of cholesterol in the egg phospholipids also difficulty is lower than 2.5%.And chemical extraction method causes certain environmental pollution again inevitably, impairs experimenter's health.
Said physical extraction method is exactly supercritical fluid extraction (SFE).
Supercutical fluid (SCF) is meant the gas at emergent pressure and the above phase region of critical temperature.Because when being in supercritical state, gas-liquid two-phase character is very approaching, to such an extent as to can't differentiate, so claim supercutical fluid (SCF).
As far back as discovery gases under supercritical state such as J.B.Hannay in 1897 solid matter is had solvency action, that is to say that supercutical fluid is the same with liquid, can dissolved solids.And this supercutical fluid is during as " solvent ", solvency action to material is stressed, Temperature Influence, reach the isolating purpose of different substances by changing temperature and pressure, so just formed said physical extraction method (supercritical fluid extraction), supercritical extraction solvent commonly used has ammonia, carbonic acid gas, butane, ethane etc.
Because carbonic acid gas (CO
2) be a kind of inactive gas.Its critical temperature (Tc:31.1 ℃) is bordering on the normal temperature level, and emergent pressure (Pc 7.30MPa) is also not really high, and have nontoxic, inexpensive, be easy to get, volatile, characteristics such as non-carcinogenesis, again not with extract generation chemical reaction.So carbonic acid gas is widely used in the supercritical fluid extraction being used for the separating substances in fields such as medicine, food, spices and makeup as the supercritical extraction solvent.As the supercritical extraction solvent many advantages are arranged with carbonic acid gas, do not contain deleterious organic solvent in the product owing to making as the supercritical extraction solvent with carbonic acid gas, free from environmental pollution.Supercritical carbon dioxide extraction is to carry out in carbon dioxide environment, under the normal temperature, can prevent product camber unsaturated fatty acids acid oxidase, has improved the quality of product, and extraction carries out with separating simultaneously, thereby has improved reaction efficiency greatly, and is simple to operate.Carbonic acid gas can recycle again, has reduced the cost of product.Its shortcoming is that fixed investment is bigger.
Increasing about the report of the extraction aspect of phosphatide in the last few years, Chinese patent literature CN1047083A (application number 89103233.9) is a raw material with soy bean mixed phosphatide, by extracting and separating Yelkin TTS and kephalin are separated, then with saltouing, dissolve absorption and technologies such as degreasing, Yelkin TTS further handled produced oral level and injection stage lecithin emulsifier.
Germany Patent document DE2,833,371 have reported and have used chemical extraction method, with yolk is the method that raw material is produced high purity lecithin, 2 kilograms of yolk are mixed with 5.5 kilograms of methyl ethers, at 28 ℃, 5.7 stirred 30 minutes under the condition of kg/cm, remove by filter protein, filtrate is evaporated under 40 ℃ condition, get 787 gram residues after removing methyl ether, press this method repeated treatments 7 times, evaporate under the condition of 10 kg/cm at 50 ℃ the back, again by 5000 rev/mins centrifugal 10 minutes, obtain the Yelkin TTS of higher degree.
It is that raw material is produced the method that purity is 90～99.0% Yelkin TTS that the Japanese documentation spy opens that flat 3-133991 reported with rough Yelkin TTS.This method is that the rough Yelkin TTS of a certain amount of raw material is packed in the injector, temperature remains on 32～70 ℃, nozzle from injector, be thread, speed with the 0.5-10 Grams Per Hour is injected in the extraction tank, be 32-70 ℃ with temperature meanwhile, pressure is to contain CO in the supercritical carbon dioxide of the supercritical carbon dioxide of 80-600 kg/cm or said temperature, pressure
2The ethanol of total amount 0.1-4% (weight percentage), acetone a kind of mixture wherein, with the 3-3000 liter/hour speed enter into extraction tank, supercritical carbon dioxide is contacted with rough Yelkin TTS, rough Yelkin TTS of raw material and supercritical carbon dioxide injected supercritical carbon dioxide 10-60 minute to extraction tank after injecting and finishing again.The advantage of this method is the purity height of the Yelkin TTS made of the technical process of producing Yelkin TTS that has, and its weak point is that the rate of recovery is low, the apparatus for feeding complexity, and not easy to operate, input speed is slow, yielding poorly in the unit time.
Purpose of the present invention just is to work out the method for extracting phosphatide from natural raw material, the feasible phospholipid purity height of making, and the rate of recovery is also high, and equipment is simplified to some extent, and easy to operate again, yield of unit time is greatly improved.
The process for refining of high-purity yolk phospholipid of the present invention, with the yolk powder is raw material, yolk powder is packed in the extractor, in the extractor that fills the raw material yolk powder, feed supercritical co, in extractor in extracting pressure 30-45MPa, triglyceride level (TG) and cholesterol (Ch) are collected in continuous extraction under temperature 35-55 ℃ the super critical condition in separator, continuous extraction is to no longer isolating till triglyceride level and the cholesterol; In the extractor that fills the yolk powder of having removed triglyceride level and cholesterol, feed and contain the alcoholic acid supercritical co, in extractor in extracting pressure 30～45MPa, continuous extraction under temperature 35-55 ℃ the super critical condition, in separator, collect the ethanolic soln of egg phospholipids, till continuous extraction to the ethanolic soln of egg phospholipids is collected fully in separator, the mol ratio of ethanol and carbonic acid gas is 1: 5～15 in containing the alcoholic acid supercritical co, and the resistates in the extractor is a protein powder.
The moisture content that generally contains in the yolk powder as raw material is below 10% (weight percentage, down together), to contain moisture content 1-10% for well, again to contain 1-5% for better.After packing into yolk powder in the extractor, in the extractor that fills the raw material yolk powder, feed supercritical co, in extractor in extracting pressure 30～45MPa, continuous extraction under temperature 35-55 ℃ the super critical condition, again with in extractor in extracting pressure 35-42MPa, continuous extraction is for well under temperature 36-48 ℃ the super critical condition.The average discharge of postcritical carbonic acid gas remain on 0.5～50 liter/be divided into good, again to remain on 2.5-20 liter/be divided into better.In separator, collect triglyceride level (TG) and cholesterol (Ch) to no longer isolating till triglyceride level and the cholesterol.Feed critical carbon dioxide triglyceride level and cholesterol are collected completely the time generally between 0.5～10 hour in separator.With triglyceride level and cholesterol separated and collected fully after, obtain triglyceride level and cholesterol product.In the extractor that fills the yolk powder of having removed triglyceride level and cholesterol, feed and contain the alcoholic acid supercritical co, in extractor in extracting pressure 30-45MPa, continuous extraction under temperature 35-55 ℃ the super critical condition, again with in extractor in extracting pressure 35～42MPa, continuous extraction is for well under temperature 36-48 ℃ the super critical condition.The average discharge that contains the alcoholic acid supercritical co remains on 0.5-50 liter/be divided into, again to remain on 2-20 liter/be divided into better.Collect the ethanolic soln of egg phospholipids in separator, it is 0.1～2 hour that the ethanolic soln of collecting egg phospholipids in separator is collected complete required time, again with 0.5-2 hour for well.Resistates is a protein powder in extractor.The mol ratio of ethanol and super carbonic acid gas is 1: 5～15 in containing the alcoholic acid supercritical co, and its mol ratio is good with 1: 6～13 again.The purity of used supercritical co be 92-100% (purity 92-100% is that to contain carbonic acid gas in the carbonic acid gas be 92-100%, percent by volume, down with), be good with 95～98%, be again the best with 99-99.5.The purity of home-made carbonic acid gas is generally 95～99.5%, can reach 99～100% purity after purifying again.Alcoholic acid content is 90～100% (weight percentage) in the used ethanol, with 95～99.7% for well.Alcoholic acid content is 99.7% in the commercially available dehydrated alcohol.
The ethanolic soln of collected egg phospholipids reclaims ethanol, and obtains the egg phospholipids solid phase prod through underpressure distillation in separator.The pressure of underpressure distillation control is 0.06～0.08MPa, and the temperature of control is 40-80 ℃.The prepared egg phospholipids of underpressure distillation carries out cryodrying in the pressure of 20-30Pa under-15～-35 ℃ the temperature.Egg phospholipids after the cryodrying is preserved under-15～40 ℃ temperature.
The carbonic acid gas that comes out from separator can reclaim, and recycles.Also can replace ethanol and supercritical co to extract egg phospholipids in the yolk powder in the method for the invention, but be good with ethanol with organic solvents such as acetone, sherwood oils.
The schematic flow sheet of supercritical fluid carbon dioxide extraction egg phospholipids is seen Fig. 1.A is used to store carbonic acid gas for the carbonic acid gas basin among Fig. 1.Carbonic acid gas among the carbonic acid gas basin A enters among the refrigeration plant F through valve switch G, carbonic acid gas is liquefied again purify.If the purity of the carbonic acid gas in the carbonic acid gas basin is 95～98% o'clock, the purity of carbonic acid gas is for can reach 99～99.5% after refrigeration plant F liquefaction again.Liquid carbon dioxide is pressurized to 30-45MPa in ram pump B, be good to be pressurized to 35-42MPa again.The flow pin is arranged on the ram pump B, and the flow by under meter control carbonic acid gas makes its flow that reaches needed carbonic acid gas, enters among the extractor C to extract, and removes triglyceride level and cholesterol in the yolk powder.Triglyceride level and cholesterol are collected among the separator D, and carbonic acid gas comes out to return among the carbonic acid gas basin A from separator D carbonic acid gas is reclaimed.
If when containing the alcoholic acid critical carbon dioxide and come the extracting and separating egg phospholipids, in properties-correcting agent pump E, ethanol is pressurized to 8～10MPa, the properties-correcting agent pump is provided with under meter, control alcoholic acid flow, form with the ethanol of requirement with from the carbonic acid gas of refrigeration plant F and to contain the alcoholic acid carbonic acid gas, the mol ratio that makes ethanol and carbonic acid gas is 1: 5～15, again with its mol ratio 1: 6～13 for well, containing the alcoholic acid carbonic acid gas enters among the ram pump B, be pressurized to 30～45MPa, again to be pressurized to 35～42MPa for well, formation contains the alcoholic acid supercritical co and enters among the extractor C, and the extracting and separating egg phospholipids is collected among the separator D egg phospholipids, carbonic acid gas is got back to the carbonic acid gas basin A from the D of separate chamber, stays the resistates protein powder in extractor C.
With 200 gram yolk powders is raw material, and with three kinds of products that technology of the present invention makes, they are triglyceride level and cholesterol, egg phospholipids, protein powder.Measure the weight of these three kinds of products and shared weight percentage sees Table 1 by analytical balance.
The weight of three kinds of products of table 1 and shared shared weight percentage (%) triglyceride level and 82.7 41.4 cholesterol egg phospholipidss, 27.7 13.9 protein powders 86.0 43.0 of weight percentage name of product weight (gram)
The content of the egg phospholipids in the yolk powder is 13.9% as can be seen from Table 1, meets the general document that contains about 14% and puts down in writing.
Measured phosphorus in the egg phospholipids that makes with technology of the present invention, egg phospholipids that chemical extraction method makes and the commercially available egg phospholipids with the phospho-molybdic acid method, measured their nitrogen content with micro-Kjeldahl determination, and having calculated the mole ratio of N/P, it the results are shown in Table 2.
The commercially available yolk phospholipid 3.49 1.85 1.196 of yolk phospholipid that the yolk phospholipid chemical extraction legal system 3.79 1.78 1.038 that the content of nitrogen and phosphorous and N/P mole ratio product P (%) N (%) N/P (mole ratio) technology system 3.77 1.71 1.003 of the present invention gets in three kinds of yolk phospholipids of table 2 gets
Annotate: the percentage ratio of P, N is weight percentage.
The analysis on Content result of phosphorus, nitrogen in three kinds of products as can be seen from Table 2.The phosphorus content value is similar to the phosphorus content value in the product that chemical extraction method makes in the product that technology of the present invention makes, and all is higher than the phosphorus content value in the commercially available prod.The N/P of the egg phospholipids of explained hereafter of the present invention (mole ratio) is very near 1.000 theoretical values.This just shows the nitrogenous compound that may exist in the egg phospholipids that chemical extraction method produces except that egg phospholipids.
The weight percentage of three kinds of product mesolecithal of table 3 phosphatide
Product calculates the commercially available egg phospholipids 86.1 102.4 of 95.4 98.8 egg phospholipidss that (%) produces by the egg phospholipids chemical extraction method of N calculating (%) technology 95.0 95.0 productions of the present invention by P
With thin layer chromatography egg phospholipids has been carried out qualitative analysis, its collection of illustrative plates is seen Fig. 2.Show that from qualitative result the egg phospholipids of producing with processing method of the present invention has four kinds of phosphatide at least: phosphatidylcholine (PC), phosphatidylethanolamine (PE), sphingomyelin (SM), lysolecithin (LPS).
The egg phospholipids that goes out with explained hereafter of the present invention with the scanning of Tianjin, island CS-930 dual wavelength TLC-scanner quantitatively, the results are shown in Table 4 behind thin-layer chromatography.
The content component average content of four kinds of phosphatide in the egg phospholipids of table 4 explained hereafter of the present invention, (%) CV, (%) PC 75.44 1.18 SM 2.82 3.14 LPS 6.64 2.50 PE 12.40 2.31
Each is unequal for the content of these four kinds of phosphatide as can be seen from Table 4, the highest with PC (phosphatidylcholine) content, account for 75.44% of egg phospholipids amount, successively be that PE (phosphatidylethanolamine) content be 12.4% thereafter, LPS (lysolecithin) is 6.64%, SM (sphingomyelin) is 2.82%, and the result that PC accounts for about 70% in this result and the reported in literature lecithin is similar.
With GC/MS method (gas chromatography-mass spectrography) Analysis and Identification the egg phospholipids sample made from technology of the present invention.Analytical results shows and contains 8 kinds of lipid acid in the sample, and they are Palmiticacid, stearic acid, Zoomeric acid, oleic acid, linolic acid, arachidonic acid, DHA, determines unsaturated fatty acids, and wherein unsaturated fatty acids accounts for 52%, and saturated fatty acid accounts for 48%.Nutrition indispensable fatty acid amount is about 20% in the unsaturated fatty acids.
By internal mark method determination in the egg phospholipids sample of explained hereafter of the present invention arachidonic acid content be 6.27%, DHA is 2.52%, and does not contain cholesterol.
The yolk phosphine liposoluble of coming out with explained hereafter of the present invention is in dehydrated alcohol, and concentration is 0.1%, measures its absorption spectrum with ultraviolet spectrophotometer, and its maximum absorption band is positioned at 214nm, and is very close with reported in literature.
With inductively coupled plasma atomic emission spectrometry and chemical determination the content of the various elements in the egg phospholipids sample that comes out with explained hereafter of the present invention, the results are shown in Table 5.
Content element term content (μ g/g) element term content (μ g/g) calcium (Ca) 181.0 nickel (Ni) 4.06 iron (Fe) 66.5 arsenic (As) 0.095 sodium (Na) 2105.0 lead (Ph) 0.178 potassium (K) 465.0 vanadium (V) 5.25 bronze medals (Cu) 2.90 mercury (Hg) 0.0046 zinc (Zn) 8.03 aluminium (Al) 63.10 manganese (Mn) 1.18 cadmiums (Cd) 0.0012 boron (B) 6.70 phosphorus (P) 37400.0 cobalts (Co) 0.57 of various elements in table 5 yolk phospholipid
The advantage of the process for refining of high-purity yolk phospholipid of the present invention just is:
1. technology of the present invention also has its own advantage except having super facing all characteristics of carbon dioxide extraction method, processing unit simplification of the present invention, especially feeder apparatus is simplified, and easy handling extracts with separating simultaneously and carries out, easy handling, product purity and rate of recovery height.The product egg phospholipids of making does not contain cholesterol and ethanol, and ethanol and carbonic acid gas can be recycled, and has reduced the cost of product.
2. the egg phospholipids that goes out with explained hereafter of the present invention is not owing to contain deleterious organic solvent, can be used for clinical and foodstuffs industry in.
3. technology of the present invention is owing to carbonic acid gas, ethanol recycle, and is free from environmental pollution, do not damage cut-and-try work personnel's health.
4. technology of the present invention can be produced triglyceride level and cholesterol, egg phospholipids and three kinds of products of protein powder, and except that egg phospholipids, other two kinds of products also have application and development to be worth, and the yolk powder raw material is fully utilized.
Fig. 1 is supercritical fluid carbon dioxide extraction egg phospholipids schematic flow sheet.
The thin layer chromatogram of the egg phospholipids that Fig. 2 extracts for supercritical fluid carbon dioxide.
PC (phosphatidylcholine), PE (phosphatidylethanolamine), SM (sphingomyelin), LPS (lysolecithin).
With following embodiment technology of the present invention is further described, will helps the further understanding to the present invention and advantage thereof, and not as a limitation of the invention, protection scope of the present invention is decided by claims.
Embodiment 1
With 150 gram yolk powders is raw material, yolk powder is packed among the extractor C, carbonic acid gas directly imports among the ram pump B through valve switch G from carbonic acid gas basin A, carbonic acid gas is pressurized to 31MPa formation supercritical co enters into extractor C, continuous extraction under the super critical condition of extracting pressure 31MPa and 50 ℃ in extractor C, in separator D, collect triglyceride level and cholesterol product, to no longer isolating till triglyceride level and the cholesterol, carbonic acid gas reclaims carbonic acid gas and obtains reclaiming in carbonic acid gas basin A from separator D.After having collected triglyceride level and cholesterol product, be 95% carbonic acid gas and directly import among the ram pump B from the ethanol that is pressurized to 8MPa among the properties-correcting agent pump E and to be pressurized to 44MPa from the purity of carbonic acid gas basin A, formation contains the alcoholic acid supercritical co and enters among the extractor C that fills the yolk powder of having removed triglyceride level and cholesterol, the mol ratio of ethanol and carbonic acid gas is 1: 5.5, in extractor C in extracting pressure 44MPa, continuous extraction under 48 ℃ the super critical condition is till the ethanolic soln that is extracted to egg phospholipids is collected among the separator D fully.Carbonic acid gas is got back to from separator D among the carbonic acid gas basin A.Residue among the extractor C is the protein powder product.Egg phospholipids is got egg phospholipids product 20.10 grams through underpressure distillation, and its phosphorus content (weight percentage, down together) is 3.76%, and the purity of egg phospholipids is 94.7%, and the rate of recovery is 95.7%.
Embodiment 2
Its equipment and operating process are with embodiment 1, only different is with 250 gram yolk powders is raw material, carbonic acid gas is pressurized to 38MPa, form supercritical co, enter into extractor C, continuous extraction under the super critical condition of extracting pressure 38MPa and 40 ℃ in extractor C, the carbonic acid gas average discharge remains on 1.5 liters/minute, obtains triglyceride level and cholesterol.From the carbonic acid gas of carbonic acid gas basin A with from the purity of properties-correcting agent pump E is that to be pressurized to mol ratio that 32MPa forms ethanol and carbonic acid gas in ram pump B be that 1: 14.5 the alcoholic acid supercritical co that contains enters into extractor C for 93% ethanol, in extracting pressure 32MPa, continuous extraction under the super critical condition that temperature is 38 ℃.The average discharge that contains the alcoholic acid supercritical co remains on 1.5 liters/minute.The ethanolic soln of collecting egg phospholipids is in separator D.Obtain product egg phospholipids 33.75 grams, its phosphorus content (weight percentage, down together) is 3.74%, and the purity of egg phospholipids is 94.2%, and the rate of recovery is 96.4%.
Embodiment 3
With water content is that 3% 200 gram yolk powders are raw material, and yolk powder is packed among the extractor C, and used carbonic acid gas is that commercially available purity is 96.5% carbonic acid gas.Purity is that 96.5% carbonic acid gas enters among the refrigeration plant F through valve switch G from carbonic acid gas basin A.Carbonic acid gas is liquefied again purifies, the purity of the carbonic acid gas after purifying is 99.5%, be purified to 99.5% carbonic acid gas and import among the ram pump B, the carbonic acid gas of purity 99.5% is pressurized to 42MPa forms supercritical co and enter into extractor C.Continuous extraction under the super critical condition of extracting pressure 42MPa and 48 ℃ in extractor C, the average discharge of carbonic acid gas remains on 4 liters/minute, extracts 6 hours, to no longer isolating triglyceride level and cholesterol.In separator D, triglyceride level (TG) and cholesterol (Ch) are collected fully.Carbonic acid gas reclaims carbonic acid gas in carbonic acid gas basin A from separator D.In properties-correcting agent pump E ethanol is pressurized to 9MPa, alcoholic acid content is 99.7% ethanol.Purity is that 96.5% carbonic acid gas enters into refrigeration plant F through valve switch G from carbonic acid gas basin A, makes CO
2Liquefaction is purified again, and making its purity through purification is 99.5% carbonic acid gas.Control from the alcoholic acid flow that is pressurized to 9MPa of properties-correcting agent pump E with make through purification its purity be mol ratio that 99.5% carbonic acid gas forms ethanol and carbonic acid gas be 1: 10 contain the alcoholic acid carbonic acid gas, entering into ram pump B is pressurized to 42MPa and forms and to contain the alcoholic acid supercritical co, enter into the extractor C that fills the yolk powder of having removed triglyceride level and cholesterol, in extractor C in extracting pressure 42MPa, continuous extraction under the super critical condition that temperature is 45 ℃, the average discharge that contains the alcoholic acid supercritical co is 5 liters/minute.Collect the ethanolic soln of egg phospholipids in separator D, collection time is 0.5 hour.Carbon dioxide recovery among the separator D is in carbonic acid gas basin A.The resistates that stays among the extractor C is a protein powder.The ethanolic soln of the egg phospholipids of collecting in separator D is in 0.07MPa, carry out underpressure distillation under 48 ℃ the temperature after, again in 25Pa, carry out cryodrying under-25 ℃ the condition, dried egg phospholipids is preserved under-40 ℃ temperature.Egg phospholipids product 27.80 grams that obtain, its phosphorus content (weight percentage, down together) is 3.83%, and the purity of egg phospholipids is 96.5%, and the rate of recovery is 99.3%.
Embodiment 4
Its equipment and operating process be with embodiment 3, and only different is with 100 gram fresh-laid egg blooms (Beijing birds, beasts and eggs factory) of water content 5% is raw material, is contained among the extractor C.The purity of used carbonic acid gas is 99.5% (production of Beijing grain distillery), liquefy through refrigeration plant F and to be purified to 100%, 100% carbonic acid gas being pressurized to 42MPa in ram pump B forms critical carbon dioxide and enters among the extractor C, continuous extraction under the super critical condition of extracting pressure 42MPa and 49 ℃ in extractor C, the average discharge of carbonic acid gas remains on 3 liters/minute, extracts 8 hours.In separator D, triglyceride level and cholesterol are collected fully.In properties-correcting agent pump E be that 95% ethanol is pressurized to 8MPa with ethanol content, is that mol ratio that 100% carbonic acid gas forms ethanol and carbonic acid gas is that 1: 8.33 the alcoholic acid carbonic acid gas that contains enters into ram pump B and is pressurized to 42MPa with ethanol with make its purity through purification, formation contains the alcoholic acid supercritical co and enters into extractor C, in extractor C in extracting pressure 42MPa, continuous extraction under the super critical condition that temperature is 42 ℃, the average discharge that contains the alcoholic acid supercritical co is 3 liters/minute.Collect the ethanolic soln of egg phospholipids in separator D, collection time is 0.7 hour.Carbon dioxide recovery among the separator D is in carbonic acid gas basin A.Staying resistates among the extractor C is protein powder, in 0.065MPa, carries out underpressure distillation under 60 ℃ the temperature, in the pressure of 20Pa, carries out cryodrying under-20 ℃ the temperature, preserves under-25 ℃ temperature.The egg phospholipids product that obtains is 14.10 grams, and its phosphorus content (weight percentage, down together) is 3.82%, and the purity of egg phospholipids is 96.2%, and the rate of recovery is 100%.
Embodiment 5
Its equipment and operation are with embodiment 3, only different is with 200 gram yolk powders of water content 7% is raw material, be contained among the extractor C, the purity of used carbonic acid gas is 95%, liquefy through refrigeration plant F and to be purified to 99%, carbonic acid gas with purity 99% in ram pump B is pressurized to 38MPa formation critical carbon dioxide, enters among the extractor C.In extractor C in extracting pressure 38MPa, continuous extraction under 55 ℃ the super critical condition, the average discharge of supercritical co is 2 liters/minute, extracts 4 hours.In separator D, triglyceride level and cholesterol are collected fully.In properties-correcting agent pump E be that 95% ethanol is pressurized to 10MPa with ethanol content, is that mol ratio that 99% carbonic acid gas forms ethanol and carbonic acid gas is that 1: 10 the alcoholic acid carbonic acid gas that contains enters into ram pump B and is pressurized to 38MPa with ethanol with make its purity through purification, formation contains the alcoholic acid supercritical co, enters into extractor C.In extractor C in extracting pressure 38MPa, continuous extraction under 55 ℃ the super critical condition, the average discharge that contains the alcoholic acid supercritical co is 2 liters/minute.Collect the ethanolic soln of egg phospholipids in separator D, collection time is 0.5 hour.Carbon dioxide recovery among the separator D is in carbonic acid gas basin A.The resistates that leaves among the extractor C is a protein powder, in 0.07MPa, carries out underpressure distillation under 45 ℃ the temperature, in 25Pa, carries out cryodrying under-30 ℃ the condition, preserves under-30 ℃ temperature.The egg phospholipids product that obtains is 27.40 grams, and its phosphorus content (weight percentage, down together) is 3.77%, and the purity of egg phospholipids is 95.0%, and the rate of recovery is 97.9%.
Embodiment 6
Its equipment and operation are with embodiment 3, only different is with 100 gram yolk powders of water content 2% is raw material, be contained among the extractor C, the purity of used carbonic acid gas is 95%, liquefy through refrigeration plant F and to be purified to 99%, carbonic acid gas with purity 99% in ram pump B is pressurized to 42MPa formation critical carbon dioxide, enters among the extractor C.In extractor C in extracting pressure 42MPa, continuous extraction under 45 ℃ the super critical condition, the average discharge of supercritical co is 2.5 liters/minute, extracts 10 hours.In separator D, triglyceride level and cholesterol are collected fully.In the properties-correcting agent pump be that 95% ethanol is pressurized to 9MPa with ethanol content, is that mol ratio that 99% carbonic acid gas forms ethanol and carbonic acid gas is that 1: 6.67 the alcoholic acid carbonic acid gas that contains enters into ram pump B with ethanol with make its purity through purification, be pressurized to 42MPa, formation contains the alcoholic acid supercritical co, enter into extractor C, in extractor C in extracting pressure 42MPa, continuous extraction under 45 ℃ the super critical condition, the average discharge that contains the alcoholic acid supercritical co is 2 liters/minute.Collect the ethanolic soln of egg phospholipids in separator D, the time of collection is 0.5 hour.The resistates that leaves among the extractor C is a protein powder.In 0.07MPa, carry out underpressure distillation under 58 ℃ the condition.In 25Pa, carry out cryodrying under-30 ℃ the condition, under-35 ℃ temperature, to preserve, the egg phospholipids product that obtains is 13.80 grams, and its phosphorus content (weight percentage, down together) is 3.79%, and the purity of egg phospholipids is 95.5%, and the rate of recovery is 98.5%.
Embodiment 7
Its equipment and operation be with embodiment 3, and only different is with the yolk powders of 200 grams of water content 4% is raw material, is contained among the extractor C.The purity of used carbonic acid gas is 95%, and liquefying through refrigeration plant F is purified to 99.5%.Carbonic acid gas with purity 99.5% in ram pump B is pressurized to 40MPa formation critical carbon dioxide, enters among the extractor C.In extractor C in extracting pressure 40MPa, continuous extraction under 45 ℃ the super critical condition.The average discharge of supercritical co is 3 liters/minute, extracts 6 hours.In separator D, triglyceride level is separated with cholesterol fully.In properties-correcting agent pump E be that 95% ethanol is pressurized to 9MPa with ethanol content.Is that mol ratio that 99.5% carbonic acid gas forms ethanol and carbonic acid gas is that 1: 10 the alcoholic acid carbonic acid gas that contains enters into ram pump B with ethanol with make its purity through purification, be pressurized to 40MPa, formation contains the alcoholic acid supercritical co and enters into extractor C.In extractor C in extracting pressure 40MPa, continuous extraction under 45 ℃ the super critical condition, the average discharge that contains the alcoholic acid supercritical co is 3 liters/minute.Collect the ethanolic soln of egg phospholipids in separator D, the time of collection is 0.5 hour.Leaving resistates in extractor C is protein powder.In 0.07MPa, carry out underpressure distillation under 50 ℃ the condition.In 25Pa, carry out cryodrying under-30 ℃ the condition.Under-35 ℃ temperature, preserve.The egg phospholipids product that obtains is 27.80 grams, and its phosphorus content (weight percentage, down together) is 3.80%, and the purity of egg phospholipids is 95.7%, and the rate of recovery is 99.3%.
Embodiment 8
Its equipment and operation are with embodiment 3.Only different is with 100 gram yolk powders of water content 6% is raw material, is contained among the extractor C.The purity of used carbonic acid gas is 95%, and liquefying through refrigeration plant F is purified to 99.5%.The carbonic acid gas of purity 99.5% being pressurized to 41MPa in ram pump B forms critical carbon dioxide and enters among the extractor C.In extractor C in extracting pressure 41MPa, continuous extraction under 46 ℃ the super critical condition, the average discharge of supercritical co is 2.5 liters/minute, extracts 4 hours.In separator D, triglyceride level is separated with cholesterol fully.In properties-correcting agent pump E, be ethanol content after 95% ethanol is pressurized to 9MPa, is the ethanol that is pressurized to 9MPa that mol ratio that 99.5% carbonic acid gas forms ethanol and carbonic acid gas is that 1: 10 the alcoholic acid carbonic acid gas that contains enters into ram pump B with make its purity through purification, be pressurized to 41MPa, formation contains the alcoholic acid supercritical co and enters into extractor C.In extractor C in extracting pressure 41MPa, continuous extraction under 46 ℃ the super critical condition.The average discharge that contains the alcoholic acid supercritical co is 2.5 liters/minute, collects the ethanolic soln of egg phospholipids in separator D, and the time of collection is 0.5 hour.The resistates that leaves in extractor C is a protein powder.In 0.07MPa, carry out underpressure distillation under 50 ℃ the condition, in 25Pa, carry out cryodrying under-30 ℃ the condition.Preserve under-35 ℃ temperature, the egg phospholipids product that obtains is 13.60 grams, and its phosphorus content (weight percentage, down together) is 3.77%, and the purity of egg phospholipids is 95.0%, and the rate of recovery is 97.1%.
Claims (16)
1. the process for refining of a high-purity yolk phospholipid, it is characterized in that, with the yolk powder is raw material, yolk powder is packed in the extractor, in the extractor that fills yolk powder, feed supercritical co, in extractor in extracting pressure 30～45MPa, continuous extraction under the super critical condition that temperature is 35～55 ℃, collect triglyceride level and cholesterol in separator, continuous extraction is to no longer isolating till triglyceride level and the cholesterol; In the extractor that fills the yolk powder of having removed triglyceride level and cholesterol, feed and contain the alcoholic acid supercritical co, in extractor in extracting pressure 30～45MPa, continuous extraction under the super critical condition that temperature is 35～55 ℃, in separator, collect the ethanolic soln of egg phospholipids, till continuous extraction to the ethanolic soln of egg phospholipids is collected fully in separator, in containing the alcoholic acid supercritical co, the mol ratio of ethanol and carbonic acid gas is 1: 5～15, and the resistates in the extractor is a protein powder.
2. according to the process for refining of a kind of high-purity yolk phospholipid of claim 1, it is characterized in that, contain moisture content below 10% (weight percentage, down with) in the raw material yolk powder.
3. according to the process for refining of a kind of high-purity yolk phospholipid of claim 2, it is characterized in that, contain moisture content 1～10% in the raw material yolk powder.
4. according to the process for refining of a kind of high-purity yolk phospholipid of claim 3, it is characterized in that, contain moisture content 1～5% in the raw material yolk powder.
5. according to the process for refining of a kind of high-purity yolk phospholipid of claim 1, it is characterized in that, in the extractor that fills the raw material yolk powder, feed supercritical co, in extractor in extracting pressure 35-42MPa, continuous extraction under the super critical condition that temperature is 36～48 ℃.
6. according to the process for refining of a kind of high-purity yolk phospholipid of claim 1, it is characterized in that, in the extractor that fills the yolk powder of having removed triglyceride level and cholesterol, feed and contain the alcoholic acid supercritical co, in extractor in extracting pressure 35-42MPa, continuous extraction under the super critical condition that temperature is 36～48 ℃.
7. according to the process for refining of a kind of high-purity yolk phospholipid of claim 1 or 6, it is characterized in that the mol ratio of ethanol and carbonic acid gas is 1: 6～13 in containing the alcoholic acid supercritical co.
8. according to the process for refining of a kind of high-purity yolk phospholipid of claim 1, it is characterized in that, the average discharge of supercritical co remain on the 0.5-50 liter/minute.
9. according to the process for refining of a kind of high-purity yolk phospholipid of claim 3, it is characterized in that, the average discharge of supercritical co remain on the 2.5-20 liter/minute.
10. according to the process for refining of a kind of high-purity yolk phospholipid of claim 1, it is characterized in that, the average discharge that contains the alcoholic acid supercritical co remain on the 0.5-50 liter/minute.
11. the process for refining according to a kind of high-purity yolk phospholipid of claim 10 is characterized in that, the average discharge that contains the alcoholic acid supercritical co remain on the 2-20 liter/minute.
12. the process for refining according to a kind of high-purity yolk phospholipid of claim 1 is characterized in that, the purity of carbonic acid gas is 92～100% (percent by volumes, down with).
13. the process for refining according to a kind of high-purity yolk phospholipid of claim 12 is characterized in that the purity of carbonic acid gas is 95～98%.
14. the process for refining according to a kind of high-purity yolk phospholipid of claim 12 is characterized in that the purity of carbonic acid gas is 99～99.5%.
15. the process for refining according to a kind of high-purity yolk phospholipid of claim 1 or 3 or 5 or 6 or 8 or 10 or 12 is characterized in that, the ethanolic soln of the egg phospholipids of collection is in 0.06～0.08MPa, underpressure distillation under temperature 40-80 ℃ the condition.
16. the process for refining according to a kind of high-purity yolk phospholipid of claim 15 is characterized in that the egg phospholipids that obtains after the underpressure distillation carries out cryodrying in 20-30Pa under-15～-35 ℃ the temperature.
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| CN96120082A CN1056375C (en) | 1996-10-15 | 1996-10-15 | Refining process for high-purity yolk phospholipid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN96120082A CN1056375C (en) | 1996-10-15 | 1996-10-15 | Refining process for high-purity yolk phospholipid |
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| CN1179426A true CN1179426A (en) | 1998-04-22 |
| CN1056375C CN1056375C (en) | 2000-09-13 |
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| CN96120082A Expired - Fee Related CN1056375C (en) | 1996-10-15 | 1996-10-15 | Refining process for high-purity yolk phospholipid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102151416A (en) * | 2011-02-25 | 2011-08-17 | 重庆市润东油脂有限公司 | Safety type critical carbon dioxide extraction process |
| CN103392969A (en) * | 2013-07-28 | 2013-11-20 | 吉林大学 | Enteral nutritional emulsion containing lecithin, and preparation method thereof |
| CN107397146A (en) * | 2017-06-22 | 2017-11-28 | 安徽王家坝生态农业有限公司 | A kind of preparation method of egg yolk polypeptide product |
| CN116268409A (en) * | 2022-12-29 | 2023-06-23 | 广州白云山汉方现代药业有限公司 | Application of egg yolk lecithin in auxiliary serum triglyceride reduction |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3536622A1 (en) * | 1985-10-15 | 1987-04-16 | Krupp Gmbh | METHOD AND DEVICE FOR OBTAINING SOLID MATERIALS FROM LIQUID MIXTURES |
| JPH03133991A (en) * | 1989-10-19 | 1991-06-07 | Green Cross Corp:The | Method for purifying lecithin |
| DE4010400C1 (en) * | 1990-03-31 | 1991-05-29 | Fried. Krupp Gmbh, 4300 Essen, De | |
| CN1035436C (en) * | 1994-03-07 | 1997-07-16 | 中国科学院山西煤炭化学研究所 | Method for extracting high-purity lecithin with supercritical CO2 |
-
1996
- 1996-10-15 CN CN96120082A patent/CN1056375C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102151416A (en) * | 2011-02-25 | 2011-08-17 | 重庆市润东油脂有限公司 | Safety type critical carbon dioxide extraction process |
| CN103392969A (en) * | 2013-07-28 | 2013-11-20 | 吉林大学 | Enteral nutritional emulsion containing lecithin, and preparation method thereof |
| CN107397146A (en) * | 2017-06-22 | 2017-11-28 | 安徽王家坝生态农业有限公司 | A kind of preparation method of egg yolk polypeptide product |
| CN116268409A (en) * | 2022-12-29 | 2023-06-23 | 广州白云山汉方现代药业有限公司 | Application of egg yolk lecithin in auxiliary serum triglyceride reduction |
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| Publication number | Publication date |
|---|---|
| CN1056375C (en) | 2000-09-13 |
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