CN105061495A - Preparation method for egg yolk lecithin - Google Patents
Preparation method for egg yolk lecithin Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- JQWAHKMIYCERGA-UHFFFAOYSA-N (2-nonanoyloxy-3-octadeca-9,12-dienoyloxypropoxy)-[2-(trimethylazaniumyl)ethyl]phosphinate Chemical compound CCCCCCCCC(=O)OC(COP([O-])(=O)CC[N+](C)(C)C)COC(=O)CCCCCCCC=CCC=CCCCCC JQWAHKMIYCERGA-UHFFFAOYSA-N 0.000 title abstract description 4
- 210000002969 egg yolk Anatomy 0.000 claims abstract description 78
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- 102000002322 Egg Proteins Human genes 0.000 claims abstract description 53
- 108010000912 Egg Proteins Proteins 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 52
- 235000013345 egg yolk Nutrition 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 238000004064 recycling Methods 0.000 claims abstract description 12
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims description 51
- 239000000284 extract Substances 0.000 claims description 20
- 239000000787 lecithin Substances 0.000 claims description 18
- 235000010445 lecithin Nutrition 0.000 claims description 18
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 17
- 241000287828 Gallus gallus Species 0.000 claims description 17
- 229940067606 lecithin Drugs 0.000 claims description 17
- 210000004681 ovum Anatomy 0.000 claims description 17
- 230000006837 decompression Effects 0.000 claims description 11
- 206010003210 Arteriosclerosis Diseases 0.000 claims description 3
- 208000024172 Cardiovascular disease Diseases 0.000 claims description 3
- 208000004930 Fatty Liver Diseases 0.000 claims description 3
- 206010019708 Hepatic steatosis Diseases 0.000 claims description 3
- 208000011775 arteriosclerosis disease Diseases 0.000 claims description 3
- 230000007177 brain activity Effects 0.000 claims description 3
- 239000003814 drug Substances 0.000 claims description 3
- 208000010706 fatty liver disease Diseases 0.000 claims description 3
- 230000002265 prevention Effects 0.000 claims description 3
- 231100000240 steatosis hepatitis Toxicity 0.000 claims description 3
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 description 38
- 239000002893 slag Substances 0.000 description 18
- 235000013601 eggs Nutrition 0.000 description 12
- 238000002203 pretreatment Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- -1 2000ml ethanol) Chemical compound 0.000 description 9
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 9
- 238000013019 agitation Methods 0.000 description 9
- 235000014103 egg white Nutrition 0.000 description 9
- 210000000969 egg white Anatomy 0.000 description 9
- 238000013467 fragmentation Methods 0.000 description 9
- 238000006062 fragmentation reaction Methods 0.000 description 9
- 238000002386 leaching Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 239000013558 reference substance Substances 0.000 description 5
- 238000000638 solvent extraction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000004811 liquid chromatography Methods 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N methyl alcohol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- PORPENFLTBBHSG-MGBGTMOVSA-N 1,2-dihexadecanoyl-sn-glycerol-3-phosphate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP(O)(O)=O)OC(=O)CCCCCCCCCCCCCCC PORPENFLTBBHSG-MGBGTMOVSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- RYCNUMLMNKHWPZ-SNVBAGLBSA-N 1-acetyl-sn-glycero-3-phosphocholine Chemical compound CC(=O)OC[C@@H](O)COP([O-])(=O)OCC[N+](C)(C)C RYCNUMLMNKHWPZ-SNVBAGLBSA-N 0.000 description 1
- JZNWSCPGTDBMEW-UHFFFAOYSA-N Glycerophosphorylethanolamin Natural products NCCOP(O)(=O)OCC(O)CO JZNWSCPGTDBMEW-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 150000008104 phosphatidylethanolamines Chemical class 0.000 description 1
- 150000003905 phosphatidylinositols Chemical class 0.000 description 1
- 229940067626 phosphatidylinositols Drugs 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- AVBGNFCMKJOFIN-UHFFFAOYSA-N triethylammonium acetate Chemical compound CC(O)=O.CCN(CC)CC AVBGNFCMKJOFIN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention provides a preparation method for egg yolk lecithin. The preparation method comprises the following steps of: (1) taking egg yolk powder, extracting egg yolk oil by use of a supercritical carbon dioxide extraction method, and removing the egg yolk oil to obtain residues; and (2) adding 90% ethanol, 4-8 times v/w the amount of the residues, into the residues obtained in the step (1), extracting for 3-4 times at the temperature of 30 DEG C, each for 1-1.5 h, combining filtrate, and recycling the ethanol under reduced pressure, thereby obtaining the egg yolk lecithin.
Description
Technical field
The present invention relates to a kind of preparation method and its usage of Ovum Gallus domesticus Flavus lecithin.
Background technology
Yelkin TTS (lecithin) a kind ofly distributes very wide in phospholipid in animals and plants, and its main component has phosphatidylcholine (PC), kephalin (PE), lipositol (PI) and phosphatidic acid (PA).Yelkin TTS has high nutrition and medical value, there is delaying senility, improve brain activity, prevent and treat arteriosclerosis, remove cardiovascular disorder, different physiological roles such as prevention fatty liver, skin care etc., also there is good emulsifying effect and antioxidant property simultaneously.Therefore, Yelkin TTS is extensive in sector applications such as food, medicine, makeup.The Yelkin TTS extracted in yolk becomes Ovum Gallus domesticus Flavus lecithin.
In this area, the extracting method of Yelkin TTS is generally organic solvent method of purification, supercritical CO
2extraction process, column chromatography etc.The product purity that simple organic solvent extraction explained hereafter goes out is lower, and cholesterol level is higher, the organic solvent of residual harmful in product, and its technique is more complicated, and the cost of column chromatography is high too.But, supercritical CO
2extraction as a kind of novel isolation technique, have that technique is simple, efficient low-consume energy, environmental protection, no solvent residue, selectivity high, the Yelkin TTS quality produced is high, is the advanced technologies of high-purity Ovum Gallus domesticus Flavus lecithin.
At present, supercritical CO is used
2abstraction technique prepares Ovum Gallus domesticus Flavus lecithin, is summed up and mainly contains following 3 kinds of typical processs: 1, alcohol solvent extraction+supercritical CO
2extraction; 2, supercritical CO
2extraction+alcohol solvent extraction; 3, supercritical CO
2extraction+supercritical CO
2with carry agent alcohol extraction.Wherein, in the 1st kind and the 2nd, the yield of method is relatively low, and cost is also lower, and the yield in the 3rd is relatively high, but cost is also higher.As, Gao Jin, " extraction of high-purity egg yolk lecithin, purifying and analysis and research ", Agricultural University Of Hunan, uses supercritical CO disclosed in master thesis
2extraction+alcohol solvent extraction extracts the method for Ovum Gallus domesticus Flavus lecithin, specifically by supercritical CO
2extract remainder is at 50 DEG C, and with 4,6,8,10 times amount 95% ethanol, in the water-bath of 45 DEG C, soaking 120min, yield is respectively 9.3%, 11.5%, 12.6%, 13.2%, and yield is low, and temperature is high, and cost is high.
Therefore, obtain a productive rate high, the preparation method of the Ovum Gallus domesticus Flavus lecithin that cost is low become current in the urgent need to.
Summary of the invention
An object of the present invention, provides a kind of novel method preparing Oil of egg yolk.The invention belongs to and improve invention, by existing supercritical CO
2the improvement of extraction+alcohol solvent extraction method, thus obtain unforeseeable technique effect.
The preparation method of Ovum Gallus domesticus Flavus lecithin of the present invention, comprises following concrete steps:
(1) extracting Oil of egg yolk with supercritical carbon dioxide extraction method, namely get yolk powder, is 35Mpa, CO in extracting pressure
2flow is 50L/h, extraction temperature is extract 120min under the condition of 50 DEG C, and removing Oil of egg yolk, obtains residue;
(2) in the residue of step (1), add 90% ethanol of 4-8 times amount v/w, extract 3-4 time under the condition of temperature 30 DEG C, extract 1-1.5h, merging filtrate, decompression recycling ethanol at every turn.
Wherein, v/w: refer to kg/L.
In step (2), preferably, the add-on of 90% ethanol is 4 times of residue.
In step (2), preferably, the number of times of extraction is 4 times, and each time of extracting is 1.5h.
Present invention also offers Ovum Gallus domesticus Flavus lecithin prepared by preceding method and delay senility in preparation, improve brain activity, prevent and treat arteriosclerosis, remove cardiovascular disorder, purposes in the medicine of prevention fatty liver, skin care.
Adopt the inventive method to prepare Ovum Gallus domesticus Flavus lecithin, yield is more than 16.36%, and than now, more methodical most high yield pulp1 is also high, and illustrate that the inventive method extraction efficiency is high, and the Extracting temperature of the inventive method is low, cost is low; The preferred technical scheme of the present invention, when solvent load is low, yield is up to 17.26%, with low cost, and prospects for commercial application is excellent.
Below by embodiment, the present invention is described in further details, but be not limitation of the present invention, according to foregoing of the present invention, according to ordinary technical knowledge and the customary means of this area, not departing under the present invention's above-mentioned basic fundamental thought prerequisite, the amendment of other various ways, replacement or change can also be made.
Embodiment
Experiment material and evaluation index
1. medicinal material collect, qualification and the correction of pre-treatment and plant and instrument
The Fresh Egg that this institute provides for the honest agriculture and animal husbandry Food Co., Ltd in Chengdu with egg, meets the honest fresh hen egg quality standard of Q/CZD0002S-2014 through inspection.
HA221-40-11 supercritical extraction unit Jiangsu Huaan Science Research Instrument Co., Ltd
OA2000-B digital display constant speed stirrer Shanghai Ou He mechanical means company limited
Plant and instrument verifies before use, can carry out safely, accurately to make research.
2. evaluation index
In 2.1 Ovum Gallus domesticus Flavus lecithins, main component is phosphatidylcholine, therefore, using phosphatidylcholine extract yield as evaluation index.
2.2 phosphatidylcholine content measuring methods
Measure according to high performance liquid chromatography (Chinese Pharmacopoeia annex VI D).
Chromatographic condition and system suitability silica gel are weighting agent (chromatographic column 250mm × 4.6mm, 5 μm), with methanol-water-Glacial acetic acid-triethylamine (85:15:0.45:0.05) for mobile phase A, with normal hexane-Virahol-mobile phase A (20:48:32) for Mobile phase B; Column temperature is 40 DEG C; Flow velocity is per minute 1ml, and according to the form below carries out gradient elution; Detector is light scattering detector.
Get phosphatidylethanolamine, phosphatidylinositols, phosphatidylcholine, sphingophospholipid, lyso-phosphatidylcholine reference substance are in right amount each, dissolve with trichloromethane-methyl alcohol (2:1) and quantitatively dilute and make the mixing solutions that every 1ml is 50 μ g, 100 μ g, 200 μ g, 200 μ g, 200 μ g respectively containing above-mentioned reference substance, get above-mentioned solution 20 μ l injection liquid chromatography, each composition presses said sequence wash-out successively, the peak-to-peak resolution of each composition should conform with the regulations, and number of theoretical plate calculates should be not less than 1500 by phosphatidylcholine peak.
It is appropriate that assay method precision takes phosphatidylcholine reference substance, dissolves and quantitatively dilute to make the solution in contrast product solution of every 1ml containing phosphatidylcholine 50 μ g, 100 μ g, 150 μ g, 200 μ g, 300 μ g, 400 μ g with trichloromethane-methyl alcohol (2:1).Precision measures each 20 μ l of above-mentioned reference substance solution injection liquid chromatography respectively, and record color atlas, calculates regression equation with the logarithmic value of reference substance solution concentration and corresponding peak area logarithmic value.Another precision takes this product and is about 70mg, puts in 50ml measuring bottle, and add trichloromethane-methyl alcohol (2:1) and dissolve and be diluted to scale, shake up, precision measures 20 μ l, injection liquid chromatography, record color atlas.By the content of regression equation calculation phosphatidylcholine.
The preparation method of experimental example 1 Ovum Gallus domesticus Flavus lecithin
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 4 times amount 90% ethanol (i.e. 2000ml ethanol), fixed extraction temperature 30 DEG C is extracted 4 times, each 1.5h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol.
Measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 17.23% after measured.
Get yolk powder 1000g, measure its water content≤5%, extracting pressure 35Mpa, CO2 flow 50L/h, extraction time 120min.
In triplicate, the yield of Ovum Gallus domesticus Flavus lecithin is as following table:
| Test number | 1 | 2 | 3 |
| Phosphatidylcholine yield (%) | 17.35 | 17.29 | 17.08 |
Can find out, the yield difference of the inventive method is little, and illustrate that the inventive method is stable, in addition, the average yield of the inventive method is 17.26%.
The preparation method of the yellow Yelkin TTS of experimental example 2
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 8 times amount 90% ethanol (i.e. 4000ml ethanol), fixed extraction temperature 30 DEG C is extracted 3 times, each 1h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol.
Measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 16.36% after measured.
Comparative example 1
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 4 times amount dehydrated alcohols (i.e. 2000ml ethanol), fixed extraction temperature 30 DEG C is extracted 2 times, each 1h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol, measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 9.56% after measured.
Comparative example 2
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 6 times amount dehydrated alcohols (i.e. 3000ml ethanol), fixed extraction temperature 30 DEG C is extracted 3 times, each 1.5h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol, measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 11.40% after measured.
Comparative example 3
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 8 times amount dehydrated alcohols (i.e. 4000ml ethanol), fixed extraction temperature 30 DEG C is extracted 4 times, each 2h (in leaching process Keep agitation, rotating speed is 150 revs/min), filter, merging filtrate, decompression recycling ethanol, measures phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, be 15.42% after measured.
Comparative example 4
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 8 times amount 95% ethanol (i.e. 4000ml ethanol), fixed extraction temperature 30 DEG C is extracted 2 times, each 1.5h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol, measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 11.94% after measured.
Comparative example 5
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 4 times amount 95% ethanol (i.e. 2000ml ethanol), fixed extraction temperature 30 DEG C is extracted 3 times, each 2h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol, measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 11.97% after measured.
Comparative example 6
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 6 times amount 95% ethanol (i.e. 3000ml ethanol), fixed extraction temperature 30 DEG C is extracted 4 times, each 1h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol, measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 12.28% after measured.
Comparative example 7
Pre-treatment: after egg fragmentation, divides with egg white separator and gets yolk, and in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder.Get yolk powder 1000g, measure its water content≤5%, supercritical carbon dioxide extraction method extraction Oil of egg yolk, extraction temperature is 50 DEG C, extracting pressure 35Mpa, CO
2flow 50L/h, extraction time 120min, remove Oil of egg yolk, collects residue yolk slag.
Get above-mentioned yolk slag 500g, add 6 times amount 90% ethanol (i.e. 3000ml ethanol), fixed extraction temperature 30 DEG C is extracted 2 times, each 2h (in leaching process Keep agitation, rotating speed is 150 revs/min), merging filtrate, decompression recycling ethanol, measuring phosphatidylcholine content by phosphatidylcholine content measuring method, and calculate phosphatidylcholine extract yield, is 12.55% after measured.
To sum up, under the cooperation of each special parameter in the methods of the invention, effectively can extract Ovum Gallus domesticus Flavus lecithin, yield is high, and Extracting temperature is low, and cost is low, and prospects for commercial application is good.
Claims (5)
1. a preparation method for Ovum Gallus domesticus Flavus lecithin, is characterized in that: step is as follows:
(1) get egg yolk, in 100 ~ 105 DEG C of slakings, pulverize, 70 ~ 80 DEG C are continued to be dried to moisture≤5%, pulverize, and cross No. 1 sieve, obtain yolk powder;
(2) get the yolk powder of step (1), extract Oil of egg yolk with supercritical carbon dioxide extraction method; Namely getting yolk powder, is 35Mpa, CO in extracting pressure
2flow is 50L/h, extraction temperature is extract 120min under the condition of 50 DEG C; Then remove Oil of egg yolk, obtain residue;
(3) in the residue of step (2), add 90% ethanol of 4-8 times amount v/w, extract 3-4 time under the condition of temperature 30 DEG C, extract 1-1.5h, merging filtrate, decompression recycling ethanol at every turn.
2. preparation method according to claim 1, is characterized in that: in step (3), and the add-on of 90% ethanol is preferably 4 times of residue.
3. preparation method according to claim 1, is characterized in that: in step (3), and the number of times of extraction is 4 times, and each time of extracting is 1.5h.
4. Ovum Gallus domesticus Flavus lecithin prepared by the method described in claims 1 to 3 any one.
5. Ovum Gallus domesticus Flavus lecithin described in any one of claim 1-4 delay senility in preparation, improve brain activity, prevent and treat arteriosclerosis, the purposes removed in the medicine of cardiovascular disorder, prevention fatty liver, skin care.
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| CN201510487518.7A CN105061495B (en) | 2015-08-10 | 2015-08-10 | A kind of preparation method of egg yolk lecithin |
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| CN201510487518.7A CN105061495B (en) | 2015-08-10 | 2015-08-10 | A kind of preparation method of egg yolk lecithin |
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| CN105061495A true CN105061495A (en) | 2015-11-18 |
| CN105061495B CN105061495B (en) | 2018-05-04 |
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| CN201510487518.7A Active CN105061495B (en) | 2015-08-10 | 2015-08-10 | A kind of preparation method of egg yolk lecithin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018220A (en) * | 2015-08-10 | 2015-11-04 | 四川联成迅康医药股份有限公司 | Preparation method of egg yolk oil |
| CN106977541A (en) * | 2017-05-26 | 2017-07-25 | 贝因美婴童食品股份有限公司 | A kind of method for preparing long-chain polyunsaturated fatty acid phosphatide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175581A (en) * | 1997-09-08 | 1998-03-11 | 孙传经 | Method for extracting yolk lecithin from yolk with super-critical carbon dioxide |
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2015
- 2015-08-10 CN CN201510487518.7A patent/CN105061495B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175581A (en) * | 1997-09-08 | 1998-03-11 | 孙传经 | Method for extracting yolk lecithin from yolk with super-critical carbon dioxide |
Non-Patent Citations (2)
| Title |
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| 阳东升 等: "用超临界二氧化碳萃取技术制备蛋黄卵磷脂的几种工艺探讨", 《现代化工》 * |
| 高进 等: "超临界CO2萃取蛋黄卵磷脂工艺条件的研究", 《食品工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018220A (en) * | 2015-08-10 | 2015-11-04 | 四川联成迅康医药股份有限公司 | Preparation method of egg yolk oil |
| CN106977541A (en) * | 2017-05-26 | 2017-07-25 | 贝因美婴童食品股份有限公司 | A kind of method for preparing long-chain polyunsaturated fatty acid phosphatide |
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| CN105061495B (en) | 2018-05-04 |
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