CN102965181A - Method for preparing low cholesterol high lecithin yolk oil - Google Patents

Method for preparing low cholesterol high lecithin yolk oil Download PDF

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CN102965181A
CN102965181A CN2011102596241A CN201110259624A CN102965181A CN 102965181 A CN102965181 A CN 102965181A CN 2011102596241 A CN2011102596241 A CN 2011102596241A CN 201110259624 A CN201110259624 A CN 201110259624A CN 102965181 A CN102965181 A CN 102965181A
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yolk
weight
oil
alcohol
cholesterol
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王增兴
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China Grain Products Research & Development Institute
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Abstract

The invention relates to a method for preparing low cholesterol(below 0.5wt%) high lecithin(more than 30wt%) yolk oil, which comprises the following steps: adding water with 2-3 times of yolk weight in yolk, adjusting a yolk aqueous solution with pH value of 4.0-6.0, adding 95% of alcohol so that the alcohol concentration of the yolk aqueous solution is 50wt%, centrifuging and taking sediment, adding 95% of alcohol with 4-6 times of sediment weight, repeatedly extracting for 2-3 times and collecting extraction liquid of each time, adding beta-cyclodextrine so that the concentration is 0.5%(w/v), oscillating, centrifuging to taking a supernate, and performing vacuum concentration to remove the alcohol to obtain the yolk oil. An organic solvent and a heating mode are not required for the yolk oil preparation method, the product quality can be ensured and the yield can reach 50%, so that the production cost can be reduced without usage of special equipment.

Description

The method for preparing the high Yelkin TTS Oil of egg yolk of low-cholesterol
Technical field
The present invention relates to a kind of preparation method of Oil of egg yolk, particularly a kind of method for preparing the Oil of egg yolk of low-cholesterol and high Yelkin TTS, it need not with an organic solvent reach heating, so can possess the best in quality of Oil of egg yolk.
Background technology
Egg is nutritious food, contains 12~13% protein in the egg, 11~12% fat, 1~2% inanimate matter, all the other are a small amount of VITAMIN and the carbohydrate of trace, just record in Ming Dynasty's Compendium of Material Medica " the sweet temperature of ovum oil is nontoxic, and powder applies a sore ".Contain approximately 65% neutral fat (triglyceride in the Oil of egg yolk, triglyceride), 31% Ovum Gallus domesticus Flavus lecithin (lecithin), 4% cholesterol (cholesterol), the Yelkin TTS of its contained a large amount (lecithin) is kept physiological function to health important impact (Juneja, 1997), as: it is complete to keep cytolemma, normal hepatocytes function and renal function etc., and has a prevention of arterial sclerosis, the disease of heart and liver, reduce fat and liver fat amount, the prevention gallbladdergallstonecholetithiasis, the functions such as prevention senile dementia and preventing cancer are a product that is rich in economic benefit and is worth developing.
The method that tradition is refined Oil of egg yolk is with the heating method of infusion the yolk grease to be forced out, such as United States Patent (USP) 4219544, Chinese patent CN1378785 and CN1526294, yet such heating method very easily causes the protein of yolk burned black rotten, and the health risk doubt is arranged; Japanese Patent 2004-187642 then obtains the high quality Oil of egg yolk with yolk powder through milling process, and the yolk powder after the squeezing takes out quality Oil of egg yolk in the residue with heating method again; Also use in addition solvent extration, mention with organic solvent such as ether (ethyl ether), Virahol (isopropanol) etc. such as Japanese Patent 03-052998, in conjunction with having visco-elastic material such as Vinylite (vinyl resin) extraction Oil of egg yolk; Yet the consideration on the safety of being subject to, health and the environment, selection on extraction solvent, hypotoxic organic solvent such as normal hexane (n-hexane), alcohol (alcohol) etc. have been used, the yolk powder of mentioning water content about 35% such as Japanese Patent 05-0700791 is soaked in first alcohol, heating is extruded Oil of egg yolk with milling process after removing alcohol, Japanese Patent 08-092585 is with the alcoholic extract yolk powder, Chinese patent CN1451729 contains the Oil of egg yolk of volume Yelkin TTS again with protease treatment yolk with alcoholic extract.It is different that different solvent extractions goes out the productive rate of Oil of egg yolk, the one-tenth of its Oil of egg yolk also is grouped into to some extent difference, such as normal hexane and ethyl acetate (ethyl acetate) Oil of egg yolk in the extraction feed (being ripe yolk) more effectively, its productive rate can reach more than 20%, and the composition of its lipid is as main take triglyceride; With ethanol extraction Oil of egg yolk processed then its productive rate about 8~10%, rough close with heating method, but the content of its phospholipid can reach more than 40% then obviously than normal hexane and ethyl acetate person height.The people such as Hatta (1988) deliver and utilize sodium alginate elder generation post lipoprotein, extract the technology of Oil of egg yolk from lipoprotein, the Oil of egg yolk that can make simultaneously IgY (Yolk immune globulin) and be rich in Yelkin TTS again.
The production technology of various Oil of egg yolk described above, though have to a certain degree pretty good productive rate, contain in the product too high cholesterol can't remove be must overcome problem.The technology of removing at present cholesterol in the Oil of egg yolk has many researchs, but its relative merits are arranged respectively, for example United States Patent (USP) 4333959 is mentioned the pH value that reduces fresh yolk and can be destroyed yolk emulsion stability, again with 3-5 times of weight shift out cholesterol without the cholesterol edible oil, this method can remove 89% cholesterol; Japanese Patent 11-332518 then uses the edible oil extraction cholesterol that contains 1-3% alcohol, but because this kind mode will produce the edible oil that contains in a large number cholesterol, reclaiming edible oil needs specific installation; Lin Yihui (1977) is once with paper " cycloheptaamylose carries out the condition that removes of cholesterol in the egg yolk and inquires into ", found that cholesterol and crude lecithin content can reduce respectively 94.3% and 28.9%, but this method cholesterol level still reaches 5.7%, and lecithin content is low; Chinese patent CN101538278 adopts alcohol extraction, and cyclodextrine removes cholesterol and separates yolk wet goods combination technique with deepfreeze, isolate high-purity egg yolk lecithin from yolk, but this method still contains the cholesterol below 5%; Use supercritical carbon dioxide extraction method (Supercritical carbon dioxide extraction is also arranged in recent years, SFC), such as Japanese Patent 03-206867, Chinese patent CN1476783 and CN1439700, the people such as nineteen ninety-five Bringe make low-cholesterol yolk with supercritical carbon dioxide extraction method, but the shortcoming of this method to be cost of equipment high and can't volume production.
Citing document:
1.Sungino H,Nitoda T and Juneja LR.(1997)General chemical composition of hen eggs.In:Hen eggs:Their basic and applied science.Yammamoti T,Juneja LR,Hatta H and Kim M(Eds).CRC Press.Juneja LR.1997.Egg yolk lipids.Hen eggs:their basic and applied science.Chapter 6:73-98.
2.Hatta,H.,SIM,J.and Nakai,S.(1988),Separation of Phospholipids from Egg Yolk and Recovery of Water-Soluble Proteins.Journal of Food Science53(2):425-427.
3. woods should intelligent (1997), (β-Cyclodextrin), quiet should university's food science be Master's thesis to Investigations on the Removal of Cholesterol from Chicken Egg Yolk by to remove the discussion of cholesterol in the egg yolk with cycloheptaamylose.
4.Bringe,N.A.,Howard,D.B.,and Clark,D.R.1995.Emulsifying properties of low fat,low cholesterol egg yolk prepared by supercritical CO2 extraction.Journal of Food Science 61(1):19-23.
Summary of the invention
Because existing Oil of egg yolk technology of preparing as mentioned above, no matter be heating method, milling process or solvent extration, the problem that all has cholesterol to remove, but efficient low, the high problems such as high Yelkin TTS of maybe can't possessing of cost then of the preparation method with Cholesterol removal; Therefore, the primary solution of the present invention is that existing Oil of egg yolk technology of preparing can't be effectively and the problem of Cholesterol removal cheaply.
Though but the less important solution of the present invention is existing Oil of egg yolk technology of preparing Cholesterol removal, but can't keep the problem of the high Yelkin TTS composition in the Oil of egg yolk, but though and Cholesterol removal, but must use specific installation or with an organic solvent reach type of heating, cause the problem that production cost is too high, productive rate is not good and quality product is bad.
The present invention provides a kind of method for preparing Oil of egg yolk for the problems referred to above or the disappearance that solves prior art, and its step comprises:
Yolk adds its weight 2-3 water doubly, and adjustment pH is 4.0-6.0, leaves standstill 30 minutes after fully being mixed into a yolk aqueous solution;
Adding 95% alcohol, to make the ethanol concn of the yolk aqueous solution be 50 % by weight, and the centrifuging and taking precipitation adds 95% alcohol that 4-6 doubly precipitates weight, re-extract 2-3 time;
Collect the supernatant liquor extract each time after centrifugal, add the cycloheptaamylose 45-65 ℃ concussion at least 0.5 hour that concentration is at least 0.5% (w/v), the centrifuging and taking supernatant liquor through concentrating under reduced pressure remove alcohol and an Oil of egg yolk.
According to the above-mentioned prepared Oil of egg yolk of method for preparing Oil of egg yolk, its cholesterol level is below 0.5 % by weight, and lecithin content is more than 30 % by weight, turns out to be a kind of effective ways of producing low-cholesterol, high Yelkin TTS; And the method need not be used specific installation and can reduce production costs and its productive rate can reach about fifty percent, add with an organic solvent not reach type of heating, and the quality that can possess product.Therefore, the present invention is a kind of preparation method that can improve the prior art disappearance fully and the Oil of egg yolk of superior prod quality can be provided.
The aforesaid method of the present invention, its mesolecithal are fresh yolk or liquid-type yolk or yolk powder.
The aforesaid method of the present invention is wherein adjusted the pH value of the yolk aqueous solution with alimentary acetic acid.
The aforesaid method of the present invention, wherein centrifugal is to carry out 10 minutes with 3000g.
The aforesaid method of the present invention, wherein the concentration of extraction liquid adding cycloheptaamylose is the 0.5-5 % by weight, optimum concn is 1% (w/v).
The aforesaid method of the present invention wherein adds behind the cycloheptaamylose in 60 ℃ of concussions 1 hour.
Below sincerely describe further technical characterictic of the present invention in detail with preferred embodiment.
Description of drawings
To be the present invention process the test solution state photo that the method mesolecithal aqueous solution that removes cholesterol is presented after centrifugal with acid and alcohol to Fig. 1, the oil reservoir present position of layering after wherein different ethanol concns are processed, wherein Figure 1A is that 30 % by weight ethanol concns, Figure 1B are 50 % by weight ethanol concns, and Fig. 1 C is 70 % by weight ethanol concns.
Fig. 2 is in the formed layering of the preferred embodiment of the present invention 50 % by weight ethanol concns, the TLC sheet photo of oil reservoir and water soluble protein layer, and 1 is standard substance phosphatidylcholine (PC) among the figure; 2 is oil reservoir; 3 is the lipoprotein layer.
Description of reference numerals
Among Fig. 1:
1 oil reservoir
2 water soluble protein layers
3 lipoprotein layers
Among Fig. 2:
1 phosphatidylcholine (PC)
2 oil reservoirs
3 lipoprotein layers
Embodiment
The effect of alcohol layering
The water that fresh yolk or yolk powder 5 grams add 2 times of its weight is mixed into the yolk aqueous solution, the yolk aqueous solution adds 95% alcohol again makes the ethanol concn of solution be respectively 30 % by weight, 50 % by weight and 70 % by weight, centrifugal 3000g, 10 minutes, result such as Figure 1A~1C, show the rear layering of different ethanol concns processing, the oil reservoir position is different; Figure 1A is that 30 % by weight ethanol concns, Figure 1B are 50 % by weight ethanol concns, and Fig. 1 C is 70 % by weight ethanol concns, wherein 30 effectively layerings of % by weight ethanol concn; 50-70 % by weight ethanol concn then can layering, and when 50 % by weight ethanol concn, the superiors are oil reservoir 1, sequentially is water soluble protein layer 2 and lipoprotein layer 3 down; And when 70 % by weight ethanol concn, the superiors are water soluble protein layer 2, are sequentially and down oil reservoir 1 and lipoprotein layer 3.
Oil reservoir is with thin layer chromatography (Thin layer chromatagraphy, TLC) analyze, the developping agent composition that uses and ratio are chloroform (Chloroform): methyl alcohol (Methanol): water (Water) is 65: 25: 4, developer is 10 % by weight ammonium sulfate (Ammonium sulfate), (such as Fig. 2, Lane1 is phosphatidylcholine (PC) among the figure not contain Yelkin TTS in hot-plate heating colour developing demonstration oil reservoir; Lane2 is oil reservoir; Lane3 is the lipoprotein layer).
The water soluble protein layer is with Bradford standard measure (Bradford, M.M. (1976) A rapid and sensitive method for the quantitation of microgram quantities of protein utilizing the principle of protein-dye binding.Analyt.Biochem.72,248-254. the protein stain is in conjunction with colorimetry), record the fresh yolk of 5 grams and can get 126 milligrams water soluble protein.
Result according to above alcohol layering, because the oil reservoir of 70 % by weight ethanol concns is in the position near bottom lipoprotein layer, be not easy during operation to separate with the lipoprotein layer, affect follow-up from egg white layer separation yolk grease step, therefore after balance alcohol usage quantity, accord with the cost demand with 50 % by weight ethanol concns, so following examples are all adopted 50 % by weight ethanol concns.
Acid and alcohol are processed the effect that removes cholesterol
According to precedent, fresh yolk or yolk powder 5 grams add the water of 2 times of its weight, mix, adjust pH as 4.0-6.0 take alimentary acetic acid, left standstill 30 minutes after fully mixing, with the yolk aqueous solution that forms array and be decided to be the acid adjustment treatment group, processing without acid adjustment then is control group.The above-mentioned yolk aqueous solution adds 95% alcohol again, and to make the ethanol concn of solution be 50 % by weight, centrifugal 3000g, 10 minutes, take out oil reservoir, weigh, and according to the people's such as Feng method (Feng HW, Pi CM, Wang RB, and Chen LC 1973Clinical Chemistry, Vol 19,121-122.) analyze the cholesterol of oil reservoir, result such as table 1 show that oil reservoir contains cholesterol, wherein with the pH4.5 group the highest cholesterol are arranged again, also can remove the part cholesterol by acid and alcohol processing, thereby reach the purpose of reducing cholesterol.
Table 1: the cholesterol analysis result of oil reservoir
Figure BSA00000568315300051
Prepare Oil of egg yolk and utilize cycloheptaamylose to remove the effect of cholesterol from the lipoprotein layer
Utilize above-mentioned acid and alcohol to process to remove the method for cholesterol, fresh yolk or yolk powder are added the water of 2 times of its weight, adjust the pH to 4.5 of the yolk aqueous solution with alimentary acetic acid, left standstill 30 minutes after fully mixing; The above-mentioned yolk aqueous solution adds 95% alcohol, and to make the ethanol concn of the yolk aqueous solution be 50 % by weight, through centrifugal 3000g, got precipitation in 10 minutes, 95% alcohol that adds 5 times of precipitation weight, re-extract 2 times, collect to extract each time the supernatant liquor after centrifugal and to add the cycloheptaamylose that concentration is respectively 0.5-5% (w/v) and make into array, again in 60 ℃ of concussions 1 hour, centrifugal 3000g, got supernatant liquor in 10 minutes, process its cholesterol of methods analyst described in the method that removes cholesterol with above-mentioned acid and alcohol, and with reference to the Yelkin TTS (Stewart of the methods analyst supernatant liquor of Stewart JCM, J.C.M.1980.Colorimetric determination of phospholipids with ammonium ferrothiocyanate (colorimetric method of phosphatide and sulphur cyanogen iron ammonium) .Anal.Biochem., 104,10-14), result such as table 2, show that the adding cycloheptaamylose is helpful to Cholesterol removal, and can not affect the content of Yelkin TTS.Relatively adding concentration is the removal rate 32.77 of the cycloheptaamylose of 0.5% (w/v), the removal rate of 1% (w/v) is 71.94, the removal rate of 5% (w/v) is 83.84,1% (w/v) increases by 1 times compared to the removal rate of 0.5% (w/v); Yet 5% (w/v) do not increase by 500 relatively compared to the removal rate of 1% (w/v), and therefore after considering effect and cost, preferred cycloheptaamylose working concentration is 1% (w/v).
Table 2: cycloheptaamylose removes the effect of cholesterol
Lecithin content (% by weight) Cholesterol level (mg/g) Removal rate (%)
Before the processing 64.5±2.44 17.82±1.45
0.5% (w/v) cycloheptaamylose 63.56±10.9 11.98±2.52 32.77
1.0% (w/v) cycloheptaamylose 66.73±26.04 5.00±2.05 71.94
5.0% (w/v) cycloheptaamylose 57.67±8.63 2.88±0.03 83.84
Make the preferred embodiment of the Oil of egg yolk of low-cholesterol, high Yelkin TTS
8 fresh yolk of weight 136.56 gram, fat content 36.22 grams are added the water of 2 times of its weight, adjust pH to 4.5 with alimentary acetic acid, left standstill 30 minutes after fully being mixed into the yolk aqueous solution; Adding 95% alcohol in the above-mentioned yolk aqueous solution, to make the ethanol concn of the yolk aqueous solution be 50 % by weight again, centrifugal 3000g, got precipitation in 10 minutes and add 95% alcohol that 4-6 doubly precipitates weight, re-extract 2-3 time, collect the supernatant liquor extract each time after centrifugal, the cycloheptaamylose that adds concentration 1% (w/v), in 60 ℃ of concussions 1 hour, centrifugal 3000g, got supernatant liquor in 10 minutes, and remove alcohol and make the Oil of egg yolk of a weight 19.19 grams through concentrating under reduced pressure, its Oil of egg yolk productive rate is 52.98% (19.19 ÷ 36.22 * 100%); The cholesterol level of Oil of egg yolk is 98.44mg, accounts for 0.51% of Oil of egg yolk gross weight; The lecithin content of Oil of egg yolk is 7012.81mg, accounts for 36.5% of Oil of egg yolk gross weight.
As above make in the preferred embodiment of Oil of egg yolk of low-cholesterol, high Yelkin TTS, the yolk aqueous solution of 50 % by weight ethanol concns is after centrifugal, remove again the left clear liquor of oil reservoir, and the resistates after the 95% alcoholic extract precipitation is egg yolk protein, can be as byproduct of the present invention.
Above embodiment only is explanation preferred implementation of the present invention, be not to limit interest field of the present invention, any those of ordinary skill in the art is in reference the present invention as above after the disclosed technical specification, carry out not departing from change, the modification of the technology of the present invention spirit, all be possible.Therefore, interest field of the present invention is with being as the criterion defined in the claim of the present invention.

Claims (8)

1. method for preparing Oil of egg yolk, its step comprises:
Yolk adds its weight 2-3 water doubly, and adjustment pH is 4.0-6.0, leaves standstill 30 minutes after fully being mixed into a yolk aqueous solution;
Adding 95% alcohol, to make the ethanol concn of the yolk aqueous solution be 50 % by weight, and the centrifuging and taking precipitation adds 95% alcohol that 4-6 doubly precipitates weight, re-extract 2-3 time;
Collect the supernatant liquor extract each time after centrifugal, add the cycloheptaamylose that concentration is at least 0.5 % by weight, and in 45-65 ℃ of concussion at least 0.5 hour, the centrifuging and taking supernatant liquor through concentrating under reduced pressure remove alcohol and an Oil of egg yolk.
2. method according to claim 1, wherein said yolk is fresh yolk or liquid-type yolk or yolk powder.
3. method according to claim 1 is wherein adjusted the pH value of the yolk aqueous solution with alimentary acetic acid.
4. method according to claim 1, wherein said centrifugal be to carry out 10 minutes with 3000g.
5. method according to claim 1, the concentration that wherein said extraction liquid adds behind the cycloheptaamylose is 0.5-5% (w/v).
6. method according to claim 1, the concentration that wherein said extraction liquid adds behind the cycloheptaamylose is 1% (w/v).
7. method according to claim 1 wherein, was shaken 1 hour in 60 ℃ after adding cycloheptaamylose.
8. method according to claim 1, wherein the cholesterol level of prepared Oil of egg yolk is below 0.5 % by weight, lecithin content is more than 30 % by weight.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108300567A (en) * 2018-02-07 2018-07-20 黄志成 Preparation method of no-additive egg yolk oil
TWI747486B (en) * 2020-09-10 2021-11-21 沈漢聰 Egg butter vacuum extractor and method for manufacturing egg butter

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101538278A (en) * 2009-05-11 2009-09-23 江南大学 High-purity egg yolk lecithin and production method and applications thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101538278A (en) * 2009-05-11 2009-09-23 江南大学 High-purity egg yolk lecithin and production method and applications thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
《Journal of food science》 19951231 DM Smith,et al "Cholesterol Reduction in Liquid Egg Yolk using beta-Cyclodextrin" 第60卷, 第4期 *
《食品科技》 19991231 张佳程等 beta_环糊精脱除蛋黄液中胆固醇的三种工艺流程比较 27-28 1-8 , 第04期 *
DM SMITH,ET AL: ""Cholesterol Reduction in Liquid Egg Yolk using β‐Cyclodextrin"", 《JOURNAL OF FOOD SCIENCE》, vol. 60, no. 4, 31 December 1995 (1995-12-31) *
张佳程等: "β―环糊精脱除蛋黄液中胆固醇的三种工艺流程比较", 《食品科技》, no. 04, 31 December 1999 (1999-12-31), pages 27 - 28 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108300567A (en) * 2018-02-07 2018-07-20 黄志成 Preparation method of no-additive egg yolk oil
TWI747486B (en) * 2020-09-10 2021-11-21 沈漢聰 Egg butter vacuum extractor and method for manufacturing egg butter

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Application publication date: 20130313