CN101538278B - High-purity egg yolk lecithin and production method and applications thereof - Google Patents

High-purity egg yolk lecithin and production method and applications thereof Download PDF

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Publication number
CN101538278B
CN101538278B CN2009101366300A CN200910136630A CN101538278B CN 101538278 B CN101538278 B CN 101538278B CN 2009101366300 A CN2009101366300 A CN 2009101366300A CN 200910136630 A CN200910136630 A CN 200910136630A CN 101538278 B CN101538278 B CN 101538278B
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cholesterol
obtains
weight
egg yolk
gallus domesticus
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CN101538278A (en
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杨严俊
徐榕榕
鄢茹辉
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Jiangnan University
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Jiangnan University
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Abstract

The invention relates to a method for separating high-purity egg yolk lecithin from the egg yolk by adopting combination technology such as extracting oil from ethanol, removing cholesterol by cyclodextrin, separating egg yolk oil by low-temperature refrigeration, and the like; and the invention also relates to a product which is obtained by adopting the method and the applications thereof. The invention has simple method and high product purity, thus having wide industrial production prospect.

Description

Ovum Gallus domesticus Flavus lecithin and production method thereof and their purposes
[technical field]
The present invention relates to technical field of food ingredient production, more specifically, the present invention relates to a kind of high-purity egg yolk lecithin and production method thereof and their purposes.
[background technology]
Main component has triglyceride level, a spot of free fatty acids, pigment etc. in the Oil of egg yolk.The yolk triglyceride level is human important nutritive substance, can produce a large amount of heats when the body metabolism oxidation.Because it is similar to human milk that the lipid acid of Oil of egg yolk is formed, therefore be used as the base oil in the infant formula.It also can be used as the assistant agent of the full Liposyn of the high nutrition of urgent patient, and patients ' recovery is played a significant role with earning a bare living.In addition, Oil of egg yolk also has effects such as anti-inflammatory, treatment scald.Ovum Gallus domesticus Flavus lecithin has become very universal nutritive health-care food in developed country, in many countries, Ovum Gallus domesticus Flavus lecithin has become a kind of nutritious supplementary as VITAMIN, even the food of going with rice or bread the most, and it is described as " greatest nutritionist ", " natural blood purificant ".The development of China's Ovum Gallus domesticus Flavus lecithin is also quite backward at present, output, processing unit, technology, product function and kind all can't satisfy domestic needs, the whole dependence on import of high-quality Ovum Gallus domesticus Flavus lecithin, therefore the domestic market prospect is very wide, potentiality to be exploited will be very considerable, press for develop a kind of extract high-purity egg yolk lecithin fast, the extracting method produced of economy and compliance with environmental protection requirements.The traditional extraction Oil of egg yolk and the method for Ovum Gallus domesticus Flavus lecithin are generally used organic solvent method, in Oil of egg yolk that obtains and the Ovum Gallus domesticus Flavus lecithin general owing to enrichment cholesterol influence its use, in order to overcome above-mentioned difficulties, usually need to introduce the poisonous and harmful solvent, so not only can cause organic solvent residual in product, and cause environmental pollution.The present invention continues to have quoted the organic solvent extraction method, but does not introduce the poisonous and harmful solvent in whole process of production, simultaneously successfully separately with Oil of egg yolk and Ovum Gallus domesticus Flavus lecithin, and for the production of high-purity egg yolk lecithin provides a new developing direction.
The invention still further relates to described high-purity egg yolk lecithin and have emulsification, release, dissolving, wetting, anti-oxidant, foaming, crystallization control, conjugated protein and prevent physics and chemistry functions such as age of starch, thereby can be used as emulsifying agent, antioxidant, antisticking agent, wetting agent, tenderizer, dispersion agent, remover etc. and be applied to food-processing industry.And in considerable food production, also need more high-purity egg yolk lecithin, yet but unusual difficulty of the purity that further improves Yelkin TTS.At present, people have adopted several different methods to improve its purity, (1) multiple organic solvent hybrid extraction method purity of Yelkin TTS of purifying for example, but, be easy to volatilization because common employed acetone boiling point is lower.And acetone is originally as poisonous and harmful reagent, so should not adopt.(2) supercritical carbon dioxide extraction Ovum Gallus domesticus Flavus lecithin, though its purity is very high, because overcritical installation cost is higher and energy consumption is bigger, thereby the scheme that makes becomes unacceptable.
Therefore, the inventor has carried out a large amount of intensive researchs at the defective that prior art exists, and has made the present invention finally.
[summary of the invention]
[technical problem that will solve]
The purpose of this invention is to provide a kind of high-purity egg yolk lecithin.
Another object of the present invention provides a kind of production method of high-purity egg yolk lecithin.
Another object of the present invention provides the purposes of described high-purity egg yolk lecithin.
[technical scheme]
The invention provides a kind of is raw material with the egg yolk liquid, adopt extraction using alcohol, embedding to remove the physical method combination new technology of cholesterol and for example underpressure distillation and so on, make the Ovum Gallus domesticus Flavus lecithin of the higher and good stability of purity, thereby satisfy the demand of foodstuffs industry better, also obtain by product refining cholesterin, triglyceride level and sex change concentrate egg xanthoprotein simultaneously Ovum Gallus domesticus Flavus lecithin.
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of production method of high-purity egg yolk lecithin.
The production method of described high-purity egg yolk lecithin comprises the steps:
A, ethanol lixiviate:
New fresh hen egg is checked sterilization, yolk is separated with egg white, the egg yolk liquid that obtains is according to the weight ratio 1 of described egg yolk liquid and water: the 1-3 water dilutes, should add 80-95 weight % aqueous ethanolic solution according to described dilution egg yolk liquid and aqueous ethanolic solution weight ratio 1: 7-9 by the dilution egg yolk liquid then, under temperature 40-65 ℃, carry out lixiviate 2-5 time again, each 2-5h, then, merging vat liquor filters, filtrate is standing over night at room temperature, separate insoluble triglyceride level and the sex change concentrate egg xanthoprotein remove wherein, the alcohol extract that obtains, and carry out the mensuration of cholesterol and content of triglyceride;
B, cholesterol reduction:
Add the beta-cyclodextrin aqueous solution of concentration 0.8-1.2 weight % in the alcohol extract that obtains toward step a) according to the cholesterol level of said determination, stir 10-60min down at temperature 25-65 ℃ then, carry out centrifugal 8-12min with 2000-5000r/min again, remove de-cholesterol Benexate Hydrochloride throw out, obtain the alcohol extract of cholesterol reduction;
C, underpressure distillation concentrate:
Toward step B) add water in the cholesterol reduction vat liquor that obtains in cholesterol reduction vat liquor weight 35-45%, under temperature 48-52 ℃, carried out underpressure distillation 30-60 minute, remove by filter insolubles then, the precipitation that obtains contains the Ovum Gallus domesticus Flavus lecithin in gross weight 90-98%;
The recovery of D, cholesterol and beta-cyclodextrin
At step B) the cholesterol Benexate Hydrochloride throw out water that obtains washs, carry out centrifugal 8-12min with 2000-5000r/min then, in the precipitation that obtains, add 80-95 weight % aqueous ethanolic solution, at normal pressure and 40 ℃ of-95 ℃ of following reflux 1-5h of temperature; Suction filtration while hot then, 80-95 weight % ethanol of its precipitation beta-cyclodextrin reusable heat washs, and the beta-cyclodextrin that obtains like this returns preceding step to be continued to use; The cholesterol aqueous ethanolic solution that obtains concentrates by underpressure distillation and obtains thick cholesterol, and recrystallization obtains refining cholesterin again.
A preferred embodiment of the invention, this method comprise that also employing high performance liquid chromatography-evaporat light scattering assay method is determined at step C) obtain sedimentary Ovum Gallus domesticus Flavus lecithin content.
A preferred embodiment of the invention is in steps A) under temperature 50-65 ℃, carry out lixiviate 3-5 time, each 3-4h.
In the present invention, the aqueous ethanolic solution of use 90-95 weight % aqueous ethanolic solution preferably.
According to another kind of preferred implementation of the present invention, at step B) in stir down 10-60min at temperature 50-65 ℃, carry out centrifugal 8-12min with 3000-4500r/min again.
In the present invention, described underpressure distillation concentrates to utilize and carries out at normally used in the art vacuum concentration pot.
According to another kind of preferred implementation of the present invention, at step B) in, the cholesterol level of the alcohol extract of described cholesterol reduction is in this alcohol extract gross weight below 5%.
The invention still further relates to the Ovum Gallus domesticus Flavus lecithin product that adopts aforesaid method to obtain, it is characterized in that described product is by forming in the water of this product gross weight 90-98 weight % Ovum Gallus domesticus Flavus lecithin, 1.8-2.2 weight % xenthophylls and surplus.
The invention still further relates to the purposes of described Ovum Gallus domesticus Flavus lecithin product in food and medicine.
Below the present invention will be described in more detail.
The present invention relates to the production method of high-purity egg yolk lecithin.
Those skilled in the art know, described Yelkin TTS has emulsification, release, dissolving, wetting, anti-oxidant, foaming, crystallization control, conjugated protein and prevents physics and chemistry function such as age of starch, thereby usually as emulsifying agent, antioxidant, antisticking agent, wetting agent, tenderizer, dispersion agent, remover etc.
In the present invention, described Ovum Gallus domesticus Flavus lecithin is the Yelkin TTS that is obtained by yolk, and its egg can be one or more eggs that are selected from chicken, duck, goose or other poultry, preferably, and chicken or duck's egg, more preferably egg.
In the present invention, the lecithin content that described high-purity egg yolk lecithin is construed as the Ovum Gallus domesticus Flavus lecithin product of producing is in more than this Ovum Gallus domesticus Flavus lecithin product gross weight 85 weight %, more preferably more than the 90 weight %, most preferably more than the 98 weight %.
Producing high-purity egg yolk lecithin at first is to carry out the ethanol lixiviate.
New fresh hen egg is checked sterilization, and yolk is separated with egg white.New fresh hen egg obtains yolk and egg white respectively through choosing egg, wash egg, sterilization, spraying, dry up, beat eggs, separate.Egg white can directly spray-driedly make the protein powder product, and egg yolk liquid can obtain products such as Yelkin TTS, Oil of egg yolk and remaining metaprotein respectively through separating.On meaning of the present invention, described inspection should be appreciated that it is to check whether egg is damaged, at the egg eggshell surface whether other dirt is arranged, described sterilization is to adopt common egg disinfection technology to carry out disinfection, for example adopt boiling water to soak that boiling hot, Peracetic Acid is stifling to carry out disinfection with egg disinfection technology such as formaldehyde fumigation, reach and eliminate the various microorganisms that new fresh hen egg surface exists.In the present invention, can use in the market the various the yellow and white separators of selling to carry out separating of yolk and egg white.
The egg yolk liquid that obtains is according to the weight ratio 1 of described egg yolk liquid and water: the 1-3 water dilutes, should add 80-95 weight % aqueous ethanolic solution according to described dilution egg yolk liquid and aqueous ethanolic solution weight ratio 1: 7-9 by the dilution egg yolk liquid then, under temperature 40-65 ℃, carry out lixiviate 2-5 time again, each 2-5h, then, merging vat liquor filters, filtrate is standing over night at room temperature, separate insoluble triglyceride level and the sex change concentrate egg xanthoprotein removed wherein, the alcohol extract that obtains, and carry out the mensuration of cholesterol and content of triglyceride.
In the present invention, the ethanol of use should be fermentation alcohol.The solution that described aqueous ethanolic solution is to use fermentation alcohol and distilled water preparation to obtain.In the present invention, the aqueous ethanolic solution of use 90-95 weight % aqueous ethanolic solution preferably.
A preferred embodiment of the invention, described dilution egg yolk liquid and aqueous ethanolic solution carry out lixiviate 3-5 time under temperature 50-65 ℃, each 3-4h.
In the present invention, it is that the filter plant that adopts those skilled in the art to know carries out filtering that described merging vat liquor filters, remove by filter the insoluble triglyceride level and the sex change concentrate egg xanthoprotein that exist in the alcohol extract, the filtrate alcohol extract that obtains carries out the mensuration of cholesterol and content of triglyceride again.
Described cholesterol level is to adopt rp-hplc determination.Content of triglyceride is to adopt GB15612-1995 to measure.
Then, the alcohol extract that obtains previously carries out the cholesterol reduction step again.
In the present invention, cholesterol reduction has adopted described inclusion technique, this technology is meant that a kind of molecule is embedded in the void structure of another kind of molecule, form the technology of inclusion compound, and inclusion compound is a kind of molecule to be embedded in formed mixture in the void structure of another kind of molecule by inclusion technique, therefore, this combination is not feature with the chemical bonding.
In the present invention, cyclodextrin has been used in embedding, and it is the product that starch generates after the cyclodextrin glucanotransferase effect that cultivation obtains with the basophilia genus bacillus.Be by 6-12 D-glucose molecule with 1, the cyclic oligomer sugar compounds that the 4-glycosidic link connects is water miscible irreducibility white crystals sprills, structure is a hollow circle tube.Common have α, β, a γ cyclodextrin, wherein beta-cyclodextrin is the cyclic oligomer maltose that is formed by connecting by α-(1 → 4)-glycosidic link by D-glucopyranose unit, the two ends of beta-cyclodextrin and outside are wetting ability, its inner chamber has stronger hydrophobicity, can the many inorganic and organic compound of embedding.
Generally speaking, the inclusion compound that cyclodextrin forms is generally the unit molecule inclusion compound, and therefore the usage quantity of described beta-cyclodextrin can be determined according to obtaining in the alcohol extract content of cholesterol in front.
Cholesterol level according to said determination, add the beta-cyclodextrin aqueous solution of concentration 0.8-1.2 weight % in the described alcohol extract, stir 10-60min down at temperature 25-65 ℃ then, carry out centrifugal 8-12min with 2000-5000r/min again, remove de-cholesterol Benexate Hydrochloride throw out, obtain the alcohol extract of cholesterol reduction.This treatment step can make the cholesterol level of described alcohol extract reduce more than 95%.
In the present invention, described beta-cyclodextrin be selected from the limited industrial corporation of beta-cyclodextrin, Shaanxi Liquan chemical industry that biochemical industry limited liability company of Mengzhou City Huaxing for example sells with the trade(brand)name beta-cyclodextrin produce with trade(brand)name doubly he-beta-cyclodextrin, Chemical Reagent Co., Ltd., Sinopharm Group that cyclodextrin is sold produce the beta-cyclodextrin of selling with the trade(brand)name beta-cyclodextrin.The purity of beta-cyclodextrin is more than 98% in beta-cyclodextrin product gross weight beta-cyclodextrin content normally.
According to another kind of preferred implementation of the present invention, the cholesterol reduction step is to stir 10-60min down at temperature 50-65 ℃, carries out centrifugal 8-12min with 3000-4500r/min again.
Then, the alcohol extract that obtains cholesterol reduction carries out underpressure distillation and concentrates.
Add water forward in the cholesterol reduction vat liquor that step obtains in cholesterol reduction vat liquor weight 35-45%, under temperature 48-52 ℃, carried out underpressure distillation 30-60 minute, remove by filter insolubles then, the precipitation that obtains contains the Ovum Gallus domesticus Flavus lecithin in gross weight 90-98%.Described underpressure distillation is to carry out distillatory under 0.1-0.5MPa pressure.Described insolubles mainly is the Oil of egg yolk of pigment β-Hu Luobusu, xenthophylls and trace.
This sedimentary Ovum Gallus domesticus Flavus lecithin content adopts high performance liquid chromatography-evaporat light scattering assay method to measure.
In the present invention, described underpressure distillation utilization is carried out at normally used in the art vacuum concentration pot.Vacuum concentration pot for example is that port, Jiangyin City company of abundant machine works declares occasion mechanical means company limited with trade(brand)name vacuum decompression thickener product sold with trade(brand)name NZ type vacuum decompressioning and concentrating tank product sold, Hengyang City's three standing grain medicine machines manufacturing company limited with trade(brand)name QN500-3000 spherical concentration tank product sold of series or Shanghai.
The recovery of cholesterol and beta-cyclodextrin.
The cholesterol Benexate Hydrochloride throw out water that obtains previously washs, carry out centrifugal 8-12min with 2000-5000r/min then, in the precipitation that obtains, add 80-95 weight % aqueous ethanolic solution, at normal pressure and 40 ℃ of-95 ℃ of following reflux 1-5h of temperature; Suction filtration while hot then, 80-95 weight % ethanol of its precipitation beta-cyclodextrin reusable heat washs, and obtains beta-cyclodextrin like this, and it can return preceding step and continue to use.
The cholesterol aqueous ethanolic solution that obtains previously concentrates by underpressure distillation and obtains thick cholesterol, more at room temperature in 60-90 weight % aqueous ethanolic solution recrystallization obtain refining cholesterin.
Described underpressure distillation is to carry out distillatory under 0.1-0.5MPa pressure.It for example is that port, Jiangyin City company of abundant machine works declares occasion mechanical means company limited with trade(brand)name vacuum decompression thickener product sold with trade(brand)name NZ type vacuum decompressioning and concentrating tank product sold, Hengyang City's three standing grain medicine machines manufacturing company limited with trade(brand)name QN500-3000 spherical concentration tank product sold of series or Shanghai that described underpressure distillation concentrates the equipment that uses.
The invention still further relates to the Ovum Gallus domesticus Flavus lecithin product that adopts aforesaid method to obtain, it is characterized in that described product is by forming in the water of this product gross weight 90-98 weight % Ovum Gallus domesticus Flavus lecithin, 1.8-2.2 weight % xenthophylls and surplus.
The purity of Ovum Gallus domesticus Flavus lecithin product of the present invention is stable to be reached ± and 2%.
In the present invention, stable should be appreciated that of described purity is in the production process because the deviation of processing parameter precision control causes the error of lecithin content.Described purity is stable to be to adopt statistical method to measure.
The invention still further relates to the purposes of described Ovum Gallus domesticus Flavus lecithin product in food and medicine.Described Ovum Gallus domesticus Flavus lecithin product in foodstuffs industry as the application of emulsifying agent, antioxidant, antisticking agent, wetting agent, tenderizer, dispersion agent, remover.Described Ovum Gallus domesticus Flavus lecithin strengthens emulsification, lubricates, preserves moisture, diffusion and stripping feature, can strengthen sprinkling property and ease for operation, gives baked product with good quality, shelf-lives and processing characteristics.It is that dough is regulated and matter structure activator, increases the toughness of dough, increases the viscosity of dough.It also can improve the matter structure of chemical fermentation method fabricated product, finally improves symmetry, volume, graininess, appearance and the texture of goods, helps the dough extrusion molding, and prolongation can add the duration.
The consumption of described Ovum Gallus domesticus Flavus lecithin generally is the 0.25-1% of this use raw material gross weight.
Described Ovum Gallus domesticus Flavus lecithin product has emulsification, and the effect that cuts grease can be promoted blood circulation, improves serum lipid, removes superoxide, and the cholesterol in the reduction blood and the content of neutral fat reduce the delay of fat at blood vessel.Therefore, described Ovum Gallus domesticus Flavus lecithin product has purposes widely in medicine.
In the present invention, described cholesterol level is to adopt rp-hplc determination.
The method for determination of cholesterol utilization is good linear relationship with the RPLC peak area and measures its cholesterol level in cholesterol concentration 0.1-0.8g/L scope.The rp-hplc determination condition is as follows: with C 18(5 μ m, 250mm * 4.6mm) are stationary phase, and acetonitrile-Virahol (4: 1) is a moving phase, and flow velocity is 0.5mL/min, and the detection wavelength is 210nm.This method is quick, and sensitivity is simple and easy to do, but direct quantitative.
Described content of triglyceride is to adopt GB15612-1995 to measure.
In the present invention, described Ovum Gallus domesticus Flavus lecithin content can adopt following steps to measure:
The preparation of A, sample solution and standardized solution
The preparation of sample solution: accurately take by weighing the about 0.3g of sample, it is dissolved in normal hexane-Virahol (volume ratio is 1: 1) mixed solvent, be settled to 50mL, supersound process 15min, dilution is filtered with 0.45 μ m millipore filtration, sample introduction then again.
The preparation of standardized solution: accurate weighing phosphatidylcholine PC standard substance 15mg, other processing is identical as the sample solution preparation method.
The measuring method of the high performance liquid chromatography-evaporative light scattering detection of B, Ovum Gallus domesticus Flavus lecithin (HPLC-ELSD) is as follows: with Nova-Pak Silica 60A silicagel column (3.9mm * 150mm, 4 μ m) (Waters company product) is separator column, normal hexane-Virahol-3% glacial acetic acid aqueous solution (volume ratio 35: 65: 8) is a moving phase, isocratic elution, flow velocity 1.0mL/min, 30 ℃ of column temperatures, chromatographic column before use must be earlier with more than the moving phase flushing 1h, sample size 20 μ L.The ELSD parameter is as follows: 50 ℃ of light scattering detector drift tube temperatures, atomization gas (air) pressure 350kPa.Record phosphatidylcholine PC under these conditions at the good (r of 0.16-1.61g/L scope internal linear relation 2=0.9979), the detection of this method is limited to 0.64 μ g, and precision is 3.2% (n=5), and the rate of recovery is 98.2%-128.2%.
This method is used for the mensuration of actual sample, has obtained gratifying result.This method pre-treatment is simple, and analysis speed is fast.
[beneficial effect]
The present invention has following positively effect: the present invention carries oil with alcohol extraction, cyclodextrin removes cholesterol to be separated yolk wet goods physico-chemical process and combines with deepfreeze, the purity of gained Ovum Gallus domesticus Flavus lecithin and the removal efficiency of cholesterol have greatly been improved, the highest purity of Ovum Gallus domesticus Flavus lecithin product of the present invention can reach 98%, purity stability reaches ± and 2%, thus improved the use value of Yelkin TTS.
Present method is carried out the leaching process of Oil of egg yolk and Ovum Gallus domesticus Flavus lecithin under mild conditions, avoided the oxidation of Oil of egg yolk and Ovum Gallus domesticus Flavus lecithin, keeps the natural radioactivity and the functional performance of Oil of egg yolk and Ovum Gallus domesticus Flavus lecithin to greatest extent.Therefore, gained Ovum Gallus domesticus Flavus lecithin quality product height of the present invention has broad range of food and medical applications prospect.
[embodiment]
Embodiment 1: the production of high-purity egg yolk lecithin
A, ethanol lixiviate:
Adopt boiling water to soak after choosing egg, washing egg 10 tons of new fresh hen eggs and scald sterilization, dry up, the yellow and white separating device of beating eggs, use SANOVO company to sell with the trade(brand)name beating machiae separates, and obtains yolk and protein liquid respectively.The protein liquid of gained is spray-dried about 0.68 ton of the protein powder product that makes directly.The egg yolk liquid that obtains dilutes according to 1: 2 water of weight ratio of described egg yolk liquid and water, should add 95 weight % aqueous ethanolic solutions at 1: 8 according to described dilution egg yolk liquid and aqueous ethanolic solution weight ratio by the dilution egg yolk liquid then, under 50 ℃ of temperature, carry out lixiviate 4 times again, each 2h, then, merging vat liquor filters, filtrate is standing over night at room temperature, separate insoluble triglyceride level and the sex change concentrate egg xanthoprotein removed wherein, the alcohol extract that obtains, and carry out the mensuration of cholesterol and content of triglyceride.Its cholesterol and triglyceride determination method such as the foregoing measuring method of this specification sheets.
B, cholesterol reduction:
Add the beta-cyclodextrin aqueous solution that the biochemical industry limited liability company of Mengzhou City Huaxing of concentration 1.0 weight % sells with the trade(brand)name beta-cyclodextrin in the alcohol extract that obtains toward step a) according to the cholesterol level of said determination, stir 50min down for 50 ℃ in temperature then, carry out centrifugal 10min with 4000r/min again, remove de-cholesterol Benexate Hydrochloride throw out, obtain the alcohol extract of cholesterol reduction.
C, underpressure distillation concentrate:
Toward step B) add water in the cholesterol reduction vat liquor that obtains in cholesterol reduction vat liquor weight 40%, under 50 ℃ of temperature, carried out underpressure distillation 50 minutes, remove by filter insolubles then, the precipitation that obtains (Ovum Gallus domesticus Flavus lecithin product) contains the Ovum Gallus domesticus Flavus lecithin in gross weight 95%, and the gross weight that can obtain the Ovum Gallus domesticus Flavus lecithin product altogether is 0.35 ton.The foregoing measuring method of this Ovum Gallus domesticus Flavus lecithin measuring method such as this specification sheets.
The recovery of D, cholesterol and beta-cyclodextrin
At step B) the cholesterol Benexate Hydrochloride throw out water that obtains washs, and carries out centrifugal 10min with 4000r/min then, adds 95 weight % aqueous ethanolic solutions in the precipitation that obtains, at normal pressure and 80 ℃ of following reflux 4h of temperature; Suction filtration while hot then, 95 weight % ethanol of its precipitation beta-cyclodextrin reusable heat wash, and the beta-cyclodextrin that obtains like this returns preceding step to be continued to use, and the beta-cyclodextrin gross weight of recovery is 0.036 ton.The cholesterol aqueous ethanolic solution that obtains uses the trade(brand)name NZ type vacuum decompressioning and concentrating tank of port, Jiangyin City company of abundant machine works to carry out underpressure distillation under 0.2PMa and concentrates and obtain thick cholesterol; in 70 weight % aqueous ethanolic solutions, carry out recrystallization again and obtain refining cholesterin; the cholesterol level that the method that adopts this specification sheets to describe is measured reaches 93%, and its refining cholesterin gross weight is 0.047 ton.
Embodiment 2: the production of high-purity egg yolk lecithin
A, ethanol lixiviate:
Adopt boiling water to soak after choosing egg, washing egg 10 tons of new fresh hen eggs and scald sterilization, dry up, the yellow and white separating device of beating eggs, use SANOVO company to sell with the trade(brand)name beating machiae separates, and obtains yolk and protein liquid respectively.The protein liquid of gained is spray-dried about 0.68 ton of the protein powder product that makes directly.The egg yolk liquid that obtains dilutes according to 1: 4 water of weight ratio of described egg yolk liquid and water, should add 95 weight % aqueous ethanolic solutions at 1: 8 according to described dilution egg yolk liquid and aqueous ethanolic solution weight ratio by the dilution egg yolk liquid then, under 40 ℃ of temperature, carry out lixiviate 4 times again, each 2h, then, merging vat liquor filters, filtrate is standing over night at room temperature, separate insoluble triglyceride level and the sex change concentrate egg xanthoprotein removed wherein, the alcohol extract that obtains, and carry out the mensuration of cholesterol and content of triglyceride.Its cholesterol and triglyceride determination method such as the foregoing measuring method of this specification sheets.
B, cholesterol reduction:
The Quzhou victory of adding concentration 0.8 weight % in the alcohol extract that obtains toward step a) according to the cholesterol level of said determination flies the high methoxyl pectin aqueous solution that chemical industry company limited sells with the high ester of trade(brand)name (methoxyl group) pectin, stir 50min down for 50 ℃ in temperature then, carry out centrifugal 10min with 4000r/min again, remove de-cholesterol pectin mixture throw out, obtain the alcohol extract of cholesterol reduction.
C, underpressure distillation concentrate:
Toward step B) add water in the cholesterol reduction vat liquor that obtains in cholesterol reduction vat liquor weight 40%, under 50 ℃ of temperature, carried out underpressure distillation 50 minutes, remove by filter insolubles then, the precipitation that obtains (Ovum Gallus domesticus Flavus lecithin product) contains the Ovum Gallus domesticus Flavus lecithin in gross weight 90%, and can obtain Ovum Gallus domesticus Flavus lecithin product gross weight altogether is 0.36 ton.The foregoing measuring method of this Ovum Gallus domesticus Flavus lecithin measuring method such as this specification sheets.
The recovery of D, cholesterol and high methoxyl pectin
At step B) the cholesterol pectin mixture throw out water that obtains washs, and carries out centrifugal 10min with 4000r/min then, adds 95 weight % aqueous ethanolic solutions in the precipitation that obtains, at normal pressure and 70 ℃ of following reflux 5h of temperature; Suction filtration while hot then, 95 weight % ethanol of its throw out pectin reusable heat wash, and the pectin that obtains like this returns preceding step to be continued to use, and the pectin gross weight of recovery is 0.03 ton.The cholesterol aqueous ethanolic solution that obtains uses Hengyang City's three standing grain medicine machines to make company limited to carry out underpressure distillation with the spherical concentration tank of trade(brand)name QN500-3000 series under 0.2PMa and concentrate and obtain thick cholesterol, in 70 weight % aqueous ethanolic solutions, carry out recrystallization again and obtain refining cholesterin, the cholesterol level that the method that adopts this specification sheets to describe is measured reaches 87%, and its refining cholesterin gross weight is 0.045 ton.
Application Example 1
The application of Ovum Gallus domesticus Flavus lecithin in the biscuit bakery product
The biscuit baked goods that contains chemistry leavening agent adopts existing production method to use lower protein, high-fat flour to make, when producing the biscuit baked goods, in its flour, add the Yelkin TTS for preparing in described flour weight 1% embodiment of the invention 1, the biscuit baked goods of producing reaches the balanced dispersion of fat, reduce proteinic extension, prevent the formation of gluten, obtain tasty and refreshing clear and melodious, soft mouthfeel.Meanwhile, use same flour, but do not use the Yelkin TTS of embodiment of the invention preparation, adopt same production method to produce contrast biscuit baked goods.Adopt present technique field ordinary method, the tissue products evaluation personnel of group evaluate the outward appearance of said two products, matter structure, mouthfeel etc., and its result is as shown in table 1.
The biscuit fuzzy evaluation that table 1 adds the present invention's preparation gets submeter
Figure GDA0000051354830000131
The commercially available medium-to-high grade biscuit fuzzy evaluation of table 2 gets submeter
Contrast above two is shown as can be seen: this biscuit has unique local flavor and mouthfeel, fragrance is deep and remote light, sweet sense is soft thin, pleasant impression delicate fragrance, compare with commercially available medium-to-high grade biscuit, have better acceptability, this is mainly reflected in product sensory evaluation score more than 80 minutes is being 61.67%, exceeds 34.43% of common commercially available biscuit.And this has the release function of the demoulding just because of Yelkin TTS, bakes in the process, slight crack do not occur, can avoid it slight crack to occur when stock and transportation, reduces the spoilage of product.External form is complete, and the quality delicate mouthfeel is not done, and does not stick to one's teeth, do not have thirsty sense, have the chewiness of appropriateness, have with the identical better human consumer's acceptability of expensive goods, have certain market competitiveness, replenish a kind of approach of taking in Ovum Gallus domesticus Flavus lecithin as human body simultaneously, practical.
Application Example 2
Ovum Gallus domesticus Flavus lecithin is in the cryogenic freezing Application in Food
Commitment adding at the icecream mix homogeneous obtains ice-creams 2 in the Yelkin TTS that described icecream mix weight 1% embodiment of the invention 1 prepares, can guarantee the dispersion of fat particle and the uniform distribution of other composition, the growth of may command ice crystal in deepfreeze helps sneaking into of air.In addition, Yelkin TTS also can produce synergy with other stablizer, thereby increases the combination to free-water, improves the flexibility of product tissue.The Yelkin TTS that has meanwhile carried out not adding the embodiment of the invention 1 preparation obtains ice-creams 1.Adopt present technique field ordinary method, the tissue products evaluation personnel of group evaluate the outward appearance of said two products, matter structure, mouthfeel etc., and its result is as shown in table 3.
When sensory evaluation, can replace butter flavor, ice crystal sense, firmness index commonly used respectively with milk powder flavor, soapy feeling, mouthful these three indexs of melting property respectively,, shorten evaluation time, improve the accuracy of estimating so as to reducing evaluation index.
Table 3 adopts index scoring method of inspection to using commercially available ice-creams 1 He
The appraisal result of the ice-creams 2 that test makes
Figure GDA0000051354830000141
As can be seen from Table 3: compare with ice-creams 1, this ice-creams 2 has unique local flavor and mouthfeel, and fragrance is deep and remote light, and sweet sense is soft thin, pleasant impression delicate fragrance.Just because Yelkin TTS has the function of emulsifying fat, and greasy feel descends greatly in the ice-creams 2, product quality delicate mouthfeel has with the identical human consumer's acceptability of expensive goods, has certain market competitiveness.
Application Example 3
The application of Ovum Gallus domesticus Flavus lecithin in baby formula milk powder
The infant development utmost point needs arachidonic acid and DHA, but himself lacks synthetic arachidonic enzyme, can only be by ingestion of food.Because arachidonic acid and DHA level and breast milk are approaching in the Ovum Gallus domesticus Flavus lecithin, the fatty acid balance height so be raw material with the Ovum Gallus domesticus Flavus lecithin, can play good result in the Yelkin TTS of described milk powder weight 2% embodiment of the invention 1 preparation for making infant formula.Europe digestant for baby medical association convened countries in the world infant nutrition expert forming member meeting to discuss and formulate new edition infant formula powder standard and standard in 2005, according to new edition infant formula powder international standard and standard, the ultimate standard of infant formula powder should be that the performance in each side such as growth pattern, biochemical indicator and immunity functions comprises and growing normally, as lactation breast milk baby.Infant formulas is defined as the baby during postnatal 4 to 6 months, only depends on this formula food of ingesting can satisfy its nutritional needs, and does not have safety problem in bed test and poison test.Be rich in linolenic acid in the Ovum Gallus domesticus Flavus lecithin, and linolenic acid in the Ovum Gallus domesticus Flavus lecithin/linolenic acid is than being 5-15: 1, and be that the Yelkin TTS of gross weight 1% embodiment of the invention 1 preparation will fully satisfy growing up healthy and sound of baby and grow the needs of required DHA so in infant formula powder, add in content.

Claims (8)

1. the production method of an Ovum Gallus domesticus Flavus lecithin is characterized in that this method comprises the steps:
A), ethanol lixiviate:
New fresh hen egg is checked sterilization, yolk is separated with egg white, the egg yolk liquid that obtains is according to the weight ratio 1 of described egg yolk liquid and water: the 1-3 water dilutes, should add 80-95 weight % aqueous ethanolic solution according to described dilution egg yolk liquid and aqueous ethanolic solution weight ratio 1: 7-9 by the dilution egg yolk liquid then, under temperature 40-65 ℃, carry out lixiviate 2-5 time again, each 2-5h, then, merging vat liquor filters, filtrate is standing over night at room temperature, separate insoluble triglyceride level and the sex change concentrate egg xanthoprotein remove wherein, the alcohol extract that obtains carries out the mensuration of cholesterol and content of triglyceride;
B), cholesterol reduction:
According to the cholesterol level of said determination toward steps A) add the beta-cyclodextrin aqueous solution of concentration 0.8-1.2 weight % in the alcohol extract that obtains, stir 10-60min down at temperature 25-65 ℃ then, carry out centrifugal 8-12min with 2000-5000r/min again, remove de-cholesterol Benexate Hydrochloride throw out, obtain the alcohol extract of cholesterol reduction;
C), underpressure distillation concentrates:
Toward step B) add water in the alcohol extract of the cholesterol reduction that obtains in the alcohol extract weight 35-45% of cholesterol reduction, under temperature 48-52 ℃, carried out underpressure distillation 30-60 minute, remove by filter insolubles then, the precipitation that obtains contains the Ovum Gallus domesticus Flavus lecithin in this precipitation gross weight 90-98%;
D), the recovery of cholesterol and beta-cyclodextrin
At step B) the cholesterol Benexate Hydrochloride throw out water that obtains washs, carry out centrifugal 8-12min with 2000-5000r/min then, in the precipitation that obtains, add 80-95 weight % aqueous ethanolic solution, at normal pressure and 40 ℃ of-95 ℃ of following reflux 1-5h of temperature; Suction filtration while hot then, 80-95 weight % ethanol of its precipitation beta-cyclodextrin reusable heat washs, and the beta-cyclodextrin that obtains like this returns preceding step to be continued to use; The cholesterol aqueous ethanolic solution that obtains concentrates by underpressure distillation and obtains thick cholesterol, and recrystallization obtains refining cholesterin again.
2. production method according to claim 1 is characterized in that this method comprises that also employing high performance liquid chromatography-evaporat light scattering assay method is determined at step C) obtain sedimentary Ovum Gallus domesticus Flavus lecithin content.
3. production method according to claim 1 is characterized in that this method steps A) and step D) use 90-95 weight % aqueous ethanolic solution.
4. production method according to claim 1 is characterized in that in steps A) under temperature 50-65 ℃, carry out lixiviate 3-5 time, each 3-4h.
5. production method according to claim 1 is characterized in that at step B) in stir down 10-60min at temperature 50-65 ℃, carry out centrifugal 8-12min with 3000-4500r/min again.
6. method according to claim 1 is characterized in that at step B) in, the cholesterol level of described cholesterol reduction alcohol extract is in this alcohol extract gross weight below 5%.
7. production method according to claim 1 is characterized in that at step C) in, described underpressure distillation concentrates and is to use vacuum concentration pot to carry out.
8. the purposes of Ovum Gallus domesticus Flavus lecithin product in food that production method according to claim 7 prepares.
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