CN103554174A - Extracting method of egg yolk lecithin - Google Patents
Extracting method of egg yolk lecithin Download PDFInfo
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- CN103554174A CN103554174A CN201310574910.6A CN201310574910A CN103554174A CN 103554174 A CN103554174 A CN 103554174A CN 201310574910 A CN201310574910 A CN 201310574910A CN 103554174 A CN103554174 A CN 103554174A
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 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 5
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Abstract
The invention belongs to the field of organic chemistry and provides an extracting method of egg yolk lecithin. A cooked egg yolk is extracted through adding ethanol. The method concretely comprises the steps of (1) cooking a fresh egg with water, and taking out the cooked yolk; (2) adding ethanol into the yolk, and stirring for 10-40min; (3) carrying out solid-liquid separation, taking a supernatant after the separation, and standing at the temperature of 4 DEG C below zero to 18 DEG C for 2-20h; (4) after standing, filtering to obtain a solidified product and a filtrate, and washing the solidified product by using the ethanol to obtain neutral yolk oil; (5) evaporating the filtrate obtained in the step (4) to obtain the egg yolk lecithin. By using the method provided by the invention, the lecithin in a yolk extracting solution has the extraction ratio of 8-15%, the recovery ratio of 90-95% and the purity of 90-95%.
Description
Technical field
The invention belongs to organic chemistry filed, be specifically related to a kind of method of extracting phosphoric acid ester from egg.
Background technology
Yelkin TTS has dividing of narrow sense and broad sense, and the Yelkin TTS of narrow sense refers to phosphatidylcholine (Phosphatidylcholine, PC); The Yelkin TTS of broad sense is coml " Yelkin TTS (Lecithin) ", is the mixture of various phosphatide.Yelkin TTS has different physiological roles: 1. delay body aging, remove free radical; 2. improve lipid metabolism, participate in forming cytolemma, control congee sample arteriosclerosis; 3. Cell protection film, prevents fatty liver; 4. promote nerve conduction, improve brain vigor; 5. strengthen the functions such as immunity.Yelkin TTS is applied to the industries such as medicine, food, makeup and feed.But existing Yelkin TTS extractive technique level is relatively backward, cannot carry out large-scale industrial production, pharmaceutical high-purity-lecithin needs a large amount of imports.
Natural phosphatidyl choline is extensively present in animal and plant body, more with yolk, soybean intensive amount, other also can be used for extracting Yelkin TTS as animal brain, liver, marrow, plant seed (vegetable seed, cottonseed, sunflower seeds, peanut, corn, Semen Flos Carthami etc.).According to the difference of raw material, current commercial custom is divided into Ovum Gallus domesticus Flavus lecithin, soybean lecithin and vegetable seed Yelkin TTS by Yelkin TTS, extracts phosphatide and mostly be soybean phospholipid in production, and rapeseed phosphatide relative nutritive value is lower, and Ovum Gallus domesticus Flavus lecithin exploitation is also less.Egg phospholipids and soybean phospholipid, because its source difference is by different forming.Yolk is more containing Yelkin TTS, reaches 9.4% of dry-matter gross weight.Phosphatidylcholine (Yelkin TTS) is the chief component composition of egg phospholipids, and its content in soybean phospholipid is lower.Soybean phospholipid is compared with egg phospholipids, and the most obvious feature is that in egg phospholipids, phosphatidylcholine PC content is high, the latter's content be about the former more than 3 times.
Usually said Ovum Gallus domesticus Flavus lecithin, refer to by abstraction technique, from yolk, extract containing phosphatidylcholine be main, the compositions such as phosphatidylethanolamine, phosphatidylinositols, phosphatidylserine are auxiliary mixture.The content of phosphatldylcholine is the leading indicator of weighing lecithin product quality height.High purity lecithin product typically refers to the phospholipid prod containing phosphatidylcholine 95% left and right.
As the deep processing of agricultural-food, the production of Yelkin TTS is one of Technical Development Area of current national emphasis support.The extracting method of research high-recovery and high-purity egg yolk lecithin has very large value to the application of further exploration Ovum Gallus domesticus Flavus lecithin.Patent CN 102690283A discloses a kind of method of extracting Yelkin TTS from egg yolk, in egg yolk liquid, adds ether+ethanol+acetone to extract; Patent CN 103224514A provides a kind of production technique of high-purity egg yolk lecithin, take dehydrated alcohol and the sherwood oil solution as extracting.Some investigators be take yolk powder as raw material, add acetone extraction (gold branch etc., < < Food science > > the 29th volume in 2008, the 10th phase: 257-259).Its extraction process is complicated, and solvent comprises more than two kinds, causes the purity of product and productive rate not high.
Summary of the invention
For problems of the prior art, the object of this invention is to provide a kind of extracting method of Ovum Gallus domesticus Flavus lecithin.
The technical scheme that realizes the object of the invention is:
An extracting method for Ovum Gallus domesticus Flavus lecithin, it is to add ethanol to extract in the yolk boiling.
Described extracting method, comprises step:
1) fresh egg water boils, and after egg is taken out, strips the yolk boiling standby;
2), to the ethanol that adds its 1-4 times volume in the yolk boiling, stir 10-40min;
3) solid-liquid separation, gets supernatant liquor after separation, standing 2-20h at-4 ℃ to 18 ℃;
4) standing rear filtration, obtains solidification products and filtrate; By solidification products described in alcohol flushing, get solid, obtain neutral Oil of egg yolk;
5) the filtrate evaporation that step 4) obtains, obtains Ovum Gallus domesticus Flavus lecithin.
Preferably, the yolk boiling described in is the yolk obtaining after the Fresh Egg poach 2-10min in a week.
More preferably, the yolk boiling described in is the yolk obtaining after Fresh Egg poach 7-9min.
Wherein, described step 2) ethanol in is the ethanol of mass concentration 90-99%, and temperature during described stirring is 50-70 ℃.
Wherein, in described step 3), supernatant liquor is standing 9-14h at 2 ℃ to 10 ℃.
Wherein, in described step 3), the method for solid-liquid separation is filtration or centrifugation.
Preferably, described in be filtered into press filtration, take the press filtration under filtration medium, pressure difference 0.5-2.0MPa condition of organic filter membrane; The centrifugal force of described centrifugation is that 1200-6000g(is that centrifugal acceleration is 1200-6000 times of universal gravity constant), the time is 5-15min.
Wherein, in described step 4), by temperature, be solidification products described in 2-5 ℃, the alcohol flushing of mass concentration 92-99%, ethanol quality be solidification products quality 3-5 doubly.
Wherein, in described step 5), described in be evaporated to a kind of in vacuum-evaporation, rotary evaporation, warm air drying, spontaneous evaporation method, the temperature of evaporation is 25-60 ℃.
Beneficial effect of the present invention is:
Method of the present invention, by groping of condition that yolk is extracted after different condition is processed, has determined extraction process, makes the extraction yield of Yelkin TTS in yolk extracting solution can reach 8%-15%, and the rate of recovery can reach 90%-95%, purity 90%-95%.Through contrast, find that phosphatidylcholine content that this technique obtains is all more than 88%, and the phosphatidylcholine content extracting reaches 90%-95% from the ripe yolk through boiling, higher than fresh yolk and yolk powder.This product is all widely used in fields such as biotechnology, health care and foodstuffs industry, has important scientific value and economic benefit.
The method that the present invention proposes, can also obtain neutral Oil of egg yolk when obtaining Ovum Gallus domesticus Flavus lecithin, implements the inventive method and can obtain larger economic benefit;
The method that the present invention proposes, is not used ethers and ketones solvent, and simple to operate, volatile gases is overflowed few, more useful to the producer and environment.
Accompanying drawing explanation
The thin layer scanning figure of Fig. 1 standard substance and sample;
Fig. 2 typical curve.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
Get fresh egg, with electromagnetic oven, boil, after water boil 8min, egg is taken out, egg white and yolk are separated, remaining complete yolk is standby.Measure a certain amount of boiled egg yolk and be placed in beaker, add the 95%(mass concentration of 3 times of yolk volumes) ethanol stirs with the accurate reinforcement electric mixer of JJ-1 under the condition of 60 ℃ of water-baths, rotating speed is 500rpm/min, after 15min, the centrifugal force that whizzer is set is 3000g, centrifugal 10min.The supernatant liquor obtaining after centrifugal is solidified to 12h under 5 ℃ of conditions, at 4 ℃, with quantitative paper, filter afterwards, obtain congealed prod and filtrate.By cold ethanol congealed prod for obtaining (4 ℃, 95% alcohol flushing 1-2 time, raw material (yolk): ethanol=1:4 weight ratio) rinse the neutral Oil of egg yolk of acquisition, extraction yield is 10.1%.The filtrate obtaining is obtained to Ovum Gallus domesticus Flavus lecithin through 48 ℃ of rotary evaporations.
Gained Ovum Gallus domesticus Flavus lecithin is 12.03% with respect to the extraction yield of shell egg, and the rate of recovery is that the 92.93%(mensuration rate of recovery is shown in attached 1: Yelkin TTS extraction yield and rate of recovery method of calculation in yolk).It is 91% that the purity (analytical procedure refers to attached 2) that adopts thin-layer chromatography methods analyst to measure the Yelkin TTS extracting records phosphatidylcholine content in the Ovum Gallus domesticus Flavus lecithin of embodiment 1.
Get fresh egg, with electromagnetic oven, boil, after water boil 8min, egg is taken out, egg white and yolk are separated, remaining complete yolk is standby.Measure a certain amount of boiled egg yolk and be placed in beaker, add 95% ethanol of 5 times of volumes, be 500rpm/min with the accurate reinforcement electric mixer of JJ-1 agitating speed under the condition of 55 ℃ of water-baths, 15min, 3000g afterwards, centrifugal 10min.Supernatant liquor after centrifugal is solidified to 12h under 5 ℃ of conditions, at 4 ℃, filter afterwards, obtain congealed prod and filtrate.By cold ethanol congealed prod for obtaining (4 ℃, 95% alcohol flushing 1-2 time, raw material (yolk): ethanol=1:4 weight ratio) rinses the neutral Oil of egg yolk of acquisition, by the filtrate of acquisition through 48 ℃ of rotary evaporations acquisition egg lecithins.
Gained Ovum Gallus domesticus Flavus lecithin is 13.10% with respect to the extraction yield of shell egg, and the rate of recovery is 94.56%.The content that thin layer chromatography records phosphatidylcholine in embodiment 1 Ovum Gallus domesticus Flavus lecithin is 94%.
Get fresh egg, with electromagnetic oven, boil, after water boil 8min, egg is taken out, egg white and yolk are separated, remaining complete yolk is standby.Measure a certain amount of boiled egg yolk and be placed in beaker, add 95% ethanol of 5 times of volumes, be 500rpm/min with the accurate reinforcement electric mixer of JJ-1 agitating speed under the condition of 65 ℃ of water-baths, 15min, 3000g afterwards, centrifugal 10min.Supernatant liquor after centrifugal is solidified to 12h under 2 ℃ of conditions, at 4 ℃, filter afterwards, obtain congealed prod and filtrate.By the congealed prod of acquisition with cold ethanol rinse (4 ℃, 95% alcohol flushing 1-2 time, raw material (yolk): ethanol=1:4 weight ratio) obtain neutral Oil of egg yolk, the filtrate obtaining is obtained to egg lecithins through 48 ℃ of rotary evaporations.
Gained Ovum Gallus domesticus Flavus lecithin is 10.96% with respect to the extraction yield of shell egg, and the rate of recovery is 94.21%.It is 93% (weight percent) that thin layer chromatography records phosphatidylcholine content in the Ovum Gallus domesticus Flavus lecithin of embodiment 1.
Get fresh egg, with electromagnetic oven, boil, after water boil 5min, egg is taken out, egg white and yolk are separated, remaining complete yolk is standby.Measure a certain amount of boiled egg yolk and be placed in beaker, add 95% ethanol of 4 times of volumes, under the condition of 55 ℃ of water-baths, with the accurate reinforcement electric mixer of JJ-1, stir, rotating speed is 500rpm/min15min, afterwards centrifugal 10min under 6000g centrifugal force.Supernatant liquor after centrifugal is solidified to 16h under 2 ℃ of conditions, at 4 ℃, filter afterwards, obtain congealed prod and filtrate.By cold ethanol congealed prod for obtaining (4 ℃, 95% alcohol flushing 1-2 time, raw material (yolk): ethanol=1:4 weight ratio) rinses the neutral Oil of egg yolk of acquisition, by the filtrate of acquisition through 42 ℃ of rotary evaporations acquisition egg lecithins.
Gained Ovum Gallus domesticus Flavus lecithin is 8.99% with respect to the extraction yield of shell egg, and the rate of recovery is 93.63%.It is 90% (weight percent) that thin layer chromatography records phosphatidylcholine content in the Ovum Gallus domesticus Flavus lecithin of embodiment 1.
Comparative example 1: extract with raw egg yolk
Get fresh egg, after breaking, egg white and yolk are separated, get yolk standby.Measure a certain amount of boiled egg yolk and be placed in beaker, add the 95%(mass concentration of 3 times of yolk volumes) ethanol stirs with the accurate reinforcement electric mixer of JJ-1 under the condition of water-bath, rotating speed is 500rpm/min, after 15min, the centrifugal force that whizzer is set is 3000g, centrifugal 10min.The supernatant liquor obtaining after centrifugal is solidified to 12h under 5 ℃ of conditions, at 4 ℃, with quantitative paper, filter afterwards, obtain congealed prod and filtrate.By cold ethanol congealed prod for obtaining (4 ℃, 95% alcohol flushing 1-2 time, raw material (yolk): ethanol=1:4 weight ratio) rinse the neutral Oil of egg yolk of acquisition, extraction yield 13%.Productive rate is greater than the extraction yield from ripe yolk, and the filtrate obtaining is obtained to Ovum Gallus domesticus Flavus lecithin through 48 ℃ of rotary evaporations.
Gained Ovum Gallus domesticus Flavus lecithin is 8.54% with respect to the extraction yield of shell egg, and the rate of recovery is 88.94%.Thin layer chromatography is surveyed purity, and recording phosphatidylcholine content in the Ovum Gallus domesticus Flavus lecithin making is 85% (weight percent).
Comparative example 2: extract with yolk powder
Get yolk powder (Jinjian, Beijing power powdered egg factory) and be placed in beaker, the 95%(mass concentration that adds 3 times of yolk powder volumes) water of ethanol and 15 times of volumes, under the condition of water-bath, with the accurate reinforcement electric mixer of JJ-1, stir, rotating speed is 500rpm/min, after 15min, the centrifugal force that whizzer is set is 3000g, centrifugal 10min.The supernatant liquor obtaining after centrifugal is solidified to 12h under 5 ℃ of conditions, at 4 ℃, with quantitative paper, filter afterwards, obtain congealed prod and filtrate.By cold ethanol congealed prod for obtaining (4 ℃, 95% alcohol flushing 1-2 time, raw material (yolk): ethanol=1:4 weight ratio) rinse the neutral Oil of egg yolk of acquisition, extraction yield is 29.5%.The filtrate obtaining is obtained to Ovum Gallus domesticus Flavus lecithin through 48 ℃ of rotary evaporations.
Gained Ovum Gallus domesticus Flavus lecithin is 12.42% with respect to the extraction yield of shell egg, and the rate of recovery is 65.36%.Thin layer chromatography is surveyed purity, and recording the Ovum Gallus domesticus Flavus lecithin purity making is 88% (weight percent).
Attached 1: Yelkin TTS extraction yield and rate of recovery method of calculation in yolk
The rate of recovery=[per-cent of Yelkin TTS theoretical content in the weight g * initial feed of the weight g/(initial feed of the Yelkin TTS obtaining)] * 100%
（2）
(wherein in fresh yolk, boiled egg yolk, the theoretical value of phospholipids content is 10%, and yolk powder is 19%)
Yelkin TTS extraction yield contrast in the different yolk of table 1
Attached 2
This experiment by dual wavelength sawtooth tlc scanning determination the purity of the Yelkin TTS that extracts.Purity of lecithin is measured formula:
In above formula: S
samplethe average peak area value of-representative sample point;
S
mark-represent the average peak area value of standard substance point;
V
samplethe point sample volume of-representative sample point;
V
mark-represent the point sample volume of standard substance point
Standard substance Reinheitszahl >=99%.
A. the drafting of typical curve
Accurate standard solution 1,2,3,4, the 5 μ l that draw put respectively on thin-layer silicon offset plate, with chloroform: methyl alcohol: water (65:25:4V/V) is developping agent ascending development 7cm, dries dibromothymolsulfonphthalein colour developing after taking-up, thin layer chromatography scanner scans spot, the results are shown in Figure 1.Peak 1-5 in figure: the peak of phosphatidylcholine standard substance, peak 6-7: the peak of self-control sample.
Using phosphatidylcholine point sample amount as X-coordinate, and amass as ordinate zou mapping on sharp side, obtains the typical curve of Fig. 2 phosphatidylcholine standard substance, and regression equation is: y=505.81x+264.15, and linearly dependent coefficient R2 is 0.9996, linear relationship is good.
B. the mensuration of phosphatidylcholine content in sample
The Ovum Gallus domesticus Flavus lecithin sample solution that accurate absorption solvent method makes respectively, puts on thin layer plate, and a retinue point reference substance solution, presses typical curve drops down, calculates the content of phosphatidylcholine in self-control Yelkin TTS by typical curve.Result is as shown in table 2:
The content of phosphatidylcholine in table 2 Ovum Gallus domesticus Flavus lecithin sample
Concrete case study on implementation described herein is only as the present invention's spirit and part experiment are illustrated.The technician in field of the present invention can make various modifications or supplements or adopt similar mode to substitute described concrete case study on implementation, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Claims (10)
1. an extracting method for Ovum Gallus domesticus Flavus lecithin, is characterized in that, is to add ethanol to extract in the yolk boiling.
2. extracting method according to claim 1, is characterized in that, comprises step:
1) fresh egg water boils, and after egg is taken out, strips the yolk boiling standby;
2), to the ethanol that adds its 1-4 times volume in the yolk boiling, stir 10-40min;
3) solid-liquid separation, gets supernatant liquor after separation, standing 2-20h at-4 ℃ to 18 ℃;
4) standing rear filtration, obtains solidification products and filtrate; By solidification products described in alcohol flushing, obtain neutral Oil of egg yolk;
5) the filtrate evaporation that step 4) obtains, obtains Ovum Gallus domesticus Flavus lecithin.
3. extracting method according to claim 1 and 2, is characterized in that, described in the yolk that boils be the yolk obtaining after Fresh Egg poach 2-10min.
4. extracting method according to claim 3, is characterized in that, described in the yolk that boils be the yolk obtaining after Fresh Egg poach 7-9min.
5. extracting method according to claim 2, is characterized in that, described step 2) in ethanol be the ethanol of mass concentration 90-99%, temperature during described stirring is 50-70 ℃.
6. extracting method according to claim 2, is characterized in that, in described step 3), supernatant liquor is standing 9-14h at 2 ℃ to 10 ℃.
7. according to the extracting method described in claim 2 or 6, it is characterized in that, in described step 3), the method for solid-liquid separation is for filtering or centrifugation.
8. extracting method according to claim 7, is characterized in that, described in be filtered into press filtration; The centrifugal force of described centrifugation is 1200-6000g, and the time is 5-15min.
9. extracting method according to claim 2, is characterized in that, in described step 4), by temperature, is solidification products described in 2-5 ℃, the alcohol flushing of mass concentration 92-99%, ethanol quality be yolk quality 3-5 doubly.
10. extracting method according to claim 2, is characterized in that, in described step 5), described in be evaporated to a kind of in vacuum-evaporation, rotary evaporation, warm air drying, spontaneous evaporation method, the temperature of evaporation is 25-60 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104544282A (en) * | 2014-12-30 | 2015-04-29 | 中国农业科学院农产品加工研究所 | Fishy smell removal method for egg powder |
| CN104946384A (en) * | 2015-06-11 | 2015-09-30 | 海南科技职业学院 | Extraction method of yolk oil |
| CN108300567A (en) * | 2018-02-07 | 2018-07-20 | 黄志成 | Preparation method of no-additive egg yolk oil |
| TWI696628B (en) * | 2018-10-12 | 2020-06-21 | 勤億蛋品科技股份有限公司 | Extraction method of lecithin |
| CN114088850A (en) * | 2021-11-26 | 2022-02-25 | 重庆伊诺生化制品有限公司 | Method for detecting phospholipid and cholesterol in polysaccharide |
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2013
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| 李梦龙等: "热处理对蛋黄卵磷脂提取的影响", 《中国食品学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104544282A (en) * | 2014-12-30 | 2015-04-29 | 中国农业科学院农产品加工研究所 | Fishy smell removal method for egg powder |
| CN104946384A (en) * | 2015-06-11 | 2015-09-30 | 海南科技职业学院 | Extraction method of yolk oil |
| CN108300567A (en) * | 2018-02-07 | 2018-07-20 | 黄志成 | Preparation method of no-additive egg yolk oil |
| TWI696628B (en) * | 2018-10-12 | 2020-06-21 | 勤億蛋品科技股份有限公司 | Extraction method of lecithin |
| CN114088850A (en) * | 2021-11-26 | 2022-02-25 | 重庆伊诺生化制品有限公司 | Method for detecting phospholipid and cholesterol in polysaccharide |
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