CN102863470B - Method for coproducing egg yolk lecithin, cephalin, yolk oil and low-denatured protein flour - Google Patents
Method for coproducing egg yolk lecithin, cephalin, yolk oil and low-denatured protein flour Download PDFInfo
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Abstract
The invention discloses a method for coproducing egg yolk phosphatidylcholine (PC), phosphatidyl ethanolamine (PE), egg oil and low denatured albumen powder, and relates to the food and medicine ingredient production field. The method comprises the steps of: separating egg white and yolk from fresh eggs; extracting neutral lipid in the yolk liquid by using a pulse ultrasonic auxiliary ethanol extraction technology, wherein alcohol insoluble solids are protein products; then extracting and separating yolk oil in the neutral lipid by using a subcritical fluid, and obtaining tow products of yolk oil and egg yolk PC compound; finally using a magnetic nano separation technology to specifically adsorb and separate PE in the egg yolk PC compound, and realizing efficient and rapid separation of PC and PE. The method of the invention coproduces the high-purity yolk PE, the egg oil and the albumen powder when performs high-purity yolk PC separation and purification, builds a high-valued, and fully utilized egg product industrial production technology with high extraction and strong operability, and provides technology support for the yolk comprehensive utilization.
Description
Technical field
The present invention relates to food, pharmaceutical ingredients production field, refering in particular to a kind of is raw material with yolk, adopt pulse ultrasonic wave auxiliary extraction technology, subcritical fluid extraction technology and magnetic Nano isolation technique to produce high-purity egg yolk lecithin, and synchronously achieve the coproduction exploitation of yolk cephalin, Oil of egg yolk and low sex change yolk powder.
Background technology
Egg is one of a few global food shared, its mesolecithal is that egg Middle nutrition is worth a part the abundantest, and protein content is not only high, and its amino acid composition is very similar to human body protein, be the high-quality complete protein being only second to cow's milk, its biological value is up to 96%; Secondly, be enriched in the lipid in yolk, not only containing abundant unsaturated fatty acids, and suitable linoleic acid content, contain the mankind at phospholipid compositions such as brain and the neural system indispensable Yelkin TTS of institute (PC), kephalins (PE) simultaneously, therefore, the exploitation of the bioactive ingredients such as the protein in egg yolk, lipid and PC, PE is the study hotspot of Chinese scholars always.
Because yolk moiety is complicated, be difficult to accomplish to make the best use of everything.Current research mainly concentrates on the separation and Extraction aspect of bioactive ingredients in yolk, seldom studies the comprehensive utilization of yolk.The present invention is intended to realize high-purity egg yolk PC separation and purification coproduction simultaneously PE, Oil of egg yolk and low sex change yolk powder, set up that a set of PC extraction efficiency is high, purity is high, the egg product production technique for deep processing of workable and high-valued, complete utilization, for yolk comprehensive utilization provides technical support.
High purity PC and PE refers to the phospholipid prod that content is greater than 95%.Its preparation mainly comprises purifying two steps, and at present, that has reported mainly includes machine solvent extration, the composite salt precipitator method, enzyme catalysis method, supercritical CO about phosphatide extracting method
2extraction process and column chromatography etc., be wherein most widely used, and applies for a patent maximum to surely belong to organic solvent extractionprocess and supercritical CO
2extraction process.
Chinese patent CN201110090211.5, CN97118167.5, CN02160786.9, CN200510060250.2, CN200910181427.5, CN201010291041.2 disclose the organic solvent extractionprocess of egg phospholipids, although this method output is large, but organic solvent consumption is large, the process time is long, extraction yield is low, and the organic solvent majority adopted does not meet environmental requirement, part organic solvent residual can cause food safety hidden danger in phosphatide.In order to improve the percentage extraction of this method, eliminate issuable food safety hidden danger, researchist adopts and food allows the ethanol used as solvent, adopt the means assisted extraction egg phospholipidss such as ultrasonic, disclosed in CN99808033.0, CN200610123974.4, Ovum Gallus domesticus Flavus lecithin is ultrasonic-and ethanol assisted Extraction follows the example of, but single-frequency ultrasonic intensity is comparatively strong, easily causes the serious degenerative of egg yolk protein, reduces its use value.
For the key problem in technology problem that above-mentioned organic solvent extractionprocess exists, the present invention introduces pulse ultrasonic wave Assisted Ethanol extractive technique, impulse ultrasound wave technology is compared with the ultrasonic technology of the conventional constant sound intensity, stronger to the destruction of cell walls, extraction efficiency is high, extraction temperature is lower simultaneously, all less on the denaturation degrees impact of PC and egg yolk protein.
Supercritical CO
2extraction is prepared lecithin and is also received much concern, Chinese patent CN02149172.0, CN99124381.1, CN02150144.0, CN02160786.9, CN03140389.1, CN94102372.9, CN96120082.0, CN200710067279.5, CN200910136630.0 disclose the supercritical liquid extraction technique of Ovum Gallus domesticus Flavus lecithin, but supercritical CO
2the problems such as extraction process also exists that treatment capacity is little all the time, equipment investment is large, product cost is higher, constrain its large-scale promotion in phosphatide production technique.
Subcritical fluid extraction technology is a novel extraction and isolation technique, there is nontoxic, environmental protection, the activeconstituents of non-thermal technology, reservation extract does not destroy, production capacity is large, can carry out industrialization scale operation, the advantages such as energy-conservation, running cost is low, for the extraction of yolk mesolecithal oil provides new approaches.The people such as Zhang Min report the research of sub-Critical Extraction of Egg Yolk Oil by Propane, and this method adopts drip washing technique, required solvent is easy to get, Oil of egg yolk yield is higher.But its not foot point is: (1) extraction efficiency is lower, extraction time is longer; (2) greatly, thus solvent-oil ratio consumes energy high, and easily remains.And the present invention selects propane or butane to be extraction solvent, the adverse current adopting stirring and leaching formula technique to carry out Oil of egg yolk repeats to extract, and greatly improves extraction efficiency, shortens extraction time.
In addition, in the preparation process of high purity lecithin, what report was maximum both at home and abroad surely belongs to column chromatography.Lv Xiuyang discloses the concrete grammar of mixed-bed ion exchange resin refined lecithin in its patent of invention CN1634940, key step is that yolk is through acetone degreasing, then 95% extraction using alcohol is used, cross the chromatography column of pretreated strong acid type resin and strong base mixed with resin, Yelkin TTS and the purity PC that is greater than 80% that purity is greater than 92% can be obtained respectively after vacuum concentration, freeze-drying.Although column chromatography can obtain the high purity lecithin that content is greater than 90%, but treatment capacity is very limited, cycle is long, complex steps, more difficultly realize continuous operation, and many organic solvents having certain toxicity in treating processes, will be used, dissolvent residual also limit this technology food, the applying of field of medicaments.
Adopt Complex precipitation with inorganic salts, also can realize the purifying of PC.Japanese Patent report mixes with thick egg phospholipids with 95% ethanol, then uses ZnCl
2after precipitation and centrifugal separation, collect ZnCl
2phospholipid complex, then the acetone adding cooling, steam desolventizing after agitation and filtration under nitrogen protection, can obtain the Yelkin TTS that purity reaches 99.6%.Complex precipitation with inorganic salts utilizes inorganic salt to the selectivity of phospholipid molecule, although greatly can improve the content of Yelkin TTS, can introduce metal ion in operation, affect quality product, cause metal ion pollution.
Therefore, develop applicable China's national situation, the preparation method of low cost, high purity PC and PE, and realize Oil of egg yolk simultaneously, the coproduction exploitation of de-fatted egg yolk protein powder has important economy and social value.
This patent adopts pulse ultrasonic wave Assisted Ethanol extractive technique, not only greatly can improve the extraction yield of neutral lipid, also can reduce the denaturation degrees of yolk protein simultaneously, improve its following process, utility value; In addition, in the subtractive process of Oil of egg yolk, introduce subcritical fluid extraction technology, a kind of novel extraction of subcritical fluid extraction technology and isolation technique, have nontoxic, environmental protection, the activeconstituents of reservation extract does not destroy, production capacity is large, can carry out the advantages such as industrialization scale operation, this technology is that the efficient extraction of egg phospholipids provides new approaches; Finally, in phosphatide purification step, adopt magnetic nanoparticle specific adsorption yolk PE first, realize the high efficiency separation of yolk PC and PE, purifying.
Summary of the invention
Reach to make egg yolk and make the best use of everything, the invention provides a kind of applicable China's national situation, low cost, high purity PC preparation method, and realize the coproduction working method of PE, Oil of egg yolk and low sex change yolk powder simultaneously.
The technical solution adopted for the present invention to solve the technical problems is: first carry out egg white after Fresh Egg inspection sterilization, yolk is separated, egg yolk liquid is placed in extractor and adds ethanol with pulse ultrasonic wave assisted extraction, alcohol extract obtains egg phospholipids crude extract after concentrated, alcohol insoluble solids is yolk protein product, then subcritical fluid extraction technology separation is adopted to go out Oil of egg yolk, finally be further purified with magnetic Nano isolation technique, prepare high-purity egg yolk PC and PE.
Method of the present invention, carry out according to following step:
(1) yolk, egg white are separated:first to Fresh Egg inspection, cleaning and sterilization, after broken shell, yolk, egg white are separated, after yolk stirs, obtain fresh egg yolk liquid; The condition of sterilization is in the boiling water of 95 ~ 100 DEG C, soaks 5 ~ 7 s.
(2) extraction of neutral lipid:fresh egg yolk liquid and water are diluted by weight 1:1 ~ 1:3 and joins in ultrasonic extraction tank after stirring, and the massfraction adding 1 ~ 9 times of volume in extractor is 80 ~ 95% ethanolic solns, pulse ultrasonic wave is adopted to carry out assisted extraction subsequently, to extract mixture after 0.1 ~ 1 h through centrifugal or filtering separation, repeatedly extract 1 ~ 5 time, merge alcohol extract and be yolk neutral lipid extracting solution (including egg phospholipids), wherein impulse ultrasound wave frequency 20 ~ 200 KHz, preferably 20 ~ 80 KHz; Extracting temperature 20 ~ 70 DEG C, wherein preferably 45 ~ 60 DEG C; Extraction time 10 ~ 60 min, recurrent interval 1 ~ 5 s.
(3) concentrated, dry:the yolk neutral lipid extracting solution of step (2) gained is evaporated to paste, recycling design at 40 ~ 50 DEG C, by the vacuum-drying at 50 ~ 65 DEG C of gained paste thing, obtains light yellow egg phospholipids crude extract.
(4) preparation of de-fatted egg yolk protein powder:collect the alcohol-insoluble substance after massfraction is 80 ~ 95% extraction using alcohols in step (2), then pasteurize (60 ~ 63 DEG C is carried out, 180 ~ 240 s), by spraying dry, drying conditions is inlet temperature 175 ~ 185 DEG C, air outlet temperature 75 ~ 80 DEG C, cools after powder delivery, through vibratory screening apparatus stage treatment.
(5) subcritical fluids is separated Oil of egg yolk:the Ovum Gallus domesticus Flavus lecithin crude extract that will obtain through step (3) loads extraction kettle, extraction kettle is vacuumized, utilize pressure difference to be injected in extraction kettle by solvent subcritical in solvent tank (propane or butane) and carry out stirring-type countercurrent leaching, whole extraction process completes under complete totally enclosed processing condition; Wherein extraction conditions is: extracting times 1 ~ 5 time, solid-liquid ratio 1:1 ~ 1:6, extraction time 10 ~ 120 min, stirring velocity 35 ~ 100 r/min, extraction temperature 10 ~ 90 DEG C, wherein preferably 40 ~ 60 DEG C, pressure 0.2 ~ 1.0 Mpa; After extraction terminates, collect from extract and obtain Oil of egg yolk, from extract remainder, obtain de-oiling egg phospholipids mixture (mainly comprising PC and PE).
(6) egg phospholipids mixture precipitation:first steam (or hot water) is adopted to heat extractor, and stir, Heating temperature 10 ~ 110 DEG C, stirring velocity 30 ~ 100 r/min, still pressure to be extracted drops to 0.01MPa, enables vacuum pump and carries out negative pressure evaporation, until pressure is down to – 0.09 below MPa, open extractor, discharge low temperature de-oiling egg phospholipids mixture; Butane after gasification is compressed, after condensation liquefaction, get back in solvent tank and recycle.
(7) preparation of Oil of egg yolk:collect step (5) gained Oil of egg yolk, adopt massfraction to be 80 ~ 95% alcohol solvent extractions, then NaOH alkali refining method carries out depickling process to high acid value Oil of egg yolk crude product; Wherein, the parameter of alcohol solvent extraction method is: solid-liquid ratio: 1:1 ~ 1:8 (g:mL), extraction time 10 ~ 60 min, extraction times 1 ~ 5; The processing condition of NaOH alkali refining method are: alkali lye mass concentration is 1 ~ 10%, and initial temperature is 20 ~ 60 DEG C, and final temperature is 50 ~ 65 DEG C, and the reaction times is 10 ~ 60 min.
(8) preparation of magnetic Nano carrier of separating:adopt chemical coprecipitation: be dissolved in the aqueous solution by the iron vitriol of solubility and Iron trichloride hexahydrate, the two mol ratio is 1:2 ~ 2:1, and total iron concentration is 0.01 ~ 0.5 mol/L; Mechanical stirring revolution is 200 ~ 800 r/min; Then add polyethylene glycol 6000 (PEG 6000), wherein add-on is 1/10 of total weight of iron; Control temperature is 40 ~ 70 DEG C, deoxygenation 30 min; Afterwards under mechanical stirring state, add 25% ammoniacal liquor or sodium hydroxide alkaline solution fast, make the pH >10 of reaction soln, under vigorous stirring state, cm-chitosan (CM-CTS) solution that mass concentration is 5 % is slowly added after stirring reaction 10 min, the add-on of CM-CTS solution is 1/10 of total reaction liquor capacity, after application of sample, temperature is elevated to rapidly 70 ~ 90 DEG C of reaction 30 ~ 120 min; After reaction terminates, under the effect of externally-applied magnetic field, sharp separation goes out magnetic-particle, by washed with de-ionized water for several times to remove unreacted chemical substance completely, until the pH of last solution is about 7; The magnetic carboxymethyl chitosan nano particle finally collecting black (is abbreviated as Fe
3o
4), and carry out lyophilize process (PEG+CM-CTS); Then Ca is adopted
2+to Fe
3o
4(PEG+CM-CTS) surface is modified further, and processing condition are as follows: the Fe of 1 mg/mL
3o
4(PEG+CM-CTS) nano particle respectively with the Ca of 2 mg/mL
2+solution mixes, and regulate the pH value of mixing solutions to 5.0 ~ 8.0, and under the Keep agitation state of 200 ~ 800 r/min, dynamic adsorption 30 ~ 120 min, makes it reach adsorption equilibrium, prepare Ca under the constant temperature of 25 ~ 50 DEG C
2+the affine magnetic nanoparticle of immobilized metal modified, is abbreviated as Fe
3o
4(PEG+CM-CTS)@Ca
2+, wherein provide Ca
2+may be the combination of a kind of in calcium chloride, calcium carbonate, calcium phosphate, caoxalate, calcium acetate or two kinds.
(9) separation and purification of PC, PE:employing massfraction is the precipitation egg phospholipids mixture of 80 ~ 95% dissolve with ethanol solution step (6) gained, adds Fe afterwards
3o
4(PEG+CM-CTS)@Ca
2+magnetic nanoparticle, at 0 ~ 37 DEG C of stirring reaction 10 ~ 180 min, makes the PE in phospholipid complex solution specifically be adsorbed on Fe
3o
4(PEG+CM-CTS)@Ca
2+magnetic nanoparticle surface, under the effect of externally-applied magnetic field, the magnetic nanoparticle being adsorbed with PE is separated from reaction soln, as eluent, wash-out is carried out to its magnetic carrier using any one in EDTA-2Na or 1 ~ 25% ammonia soln, collect elutriant, dialysis, concentrated, prepare high-purity PE; Carrier, after wash-out, can utilize Ca
2+solution regenerates, and realizes the recycling of magnetic carrier.
(10) decolouring of yolk PC:collect the adsorption liquid after step (9) process, and adopt the process of neutral active carbon decoloring, bleaching temperature 25 ~ 45 DEG C, discoloring agent addition 2.0 ~ 5.0%, bleaching time are 30 ~ 90 min.
advantage of the present invention:
(1) the present invention adopts pulse ultrasonic wave extractive technique, subcritical fluid extraction technology and magnetic Nano isolation technique, obtain high-purity PC, high-purity PE, the Oil of egg yolk of high-quality and de-fatted egg yolk protein powder 4 products simultaneously, achieve the high-valued complete utilization of yolk.
(2) when the present invention carries out yolk PC extraction, with harmless edible ethanol for solvent, adopt pulse ultrasonic wave Assisted Ethanol to extract, accelerate egg phospholipids dissolution rate, shorten the production cycle, the denaturation degrees of leaching process mesolecithal protein can be reduced again simultaneously.
(3) the present invention adopts subcritical fluid extraction technology to remove Oil of egg yolk, for supercritical extraction technique, device fabrication cost is low, shorten the production cycle, extraction process is all complete under complete totally enclosed processing condition, achieve zero release, without " three-waste pollution " in production, can not to environment.
(4) the present invention adopts magnetic Nano isolation technique to carry out refinement treatment to egg phospholipids mixture, achieves the high efficiency separation of PC and PE, and simple to operate, separation cycle is shorter, the specific adsorption of PE is good, and reaction conditions is gentle, has good industrial applications prospect.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
embodiment 1
By 100.0 kg Fresh Eggs, after picking egg, washing egg, through sterilization, (in the boiling water of 95 ~ 100 DEG C, immersion 5 ~ 7 is s), air-dry, is separated by egg white, obtains 28.0 kg egg yolk liquids after broken shell with egg white, yolk separating device with yolk.Add 28 L water in egg yolk liquid to dilute and after stirring, this yolk diluent is added in extractor, the massfraction adding 56 L is subsequently 80% ethanolic soln, at 20 KHz, lixiviate 10 min at 45 DEG C, recurrent interval 1 s, after extracting, vat liquor filters, filtrate discards precipitation in left at room temperature overnight and obtains yolk neutral fat vat liquor (including egg phospholipids), and paste is evaporated at 45 DEG C, recycling design, by the vacuum-drying at 55 DEG C of gained paste thing, obtain lurid Ovum Gallus domesticus Flavus lecithin crude extract 4.1 kg; Collect alcohol-insoluble substance, reduction vaporization residual ethanol solvent, by pasteurize, spraying dry, cooling, sieve powder, obtains de-fatted egg yolk protein powder 8.8 kg.
4.1 kg Ovum Gallus domesticus Flavus lecithin crude extracts are placed in subcritical abstraction still, extraction kettle is vacuumized, utilize pressure difference to inject in extraction kettle by butane subcritical in 4.1 L solvent tanks; Extraction process completes under complete totally enclosed processing condition, stirring velocity is 35 r/min, extraction temperature 40 DEG C, pressure-controlling is at 0.2 Mpa, and after extracting 120 min, mixing oil enters evaporating pot, under a reduced pressure, 50 DEG C of hot water heating precipitations, the butane of gasification is after compressor compression, and post liquefaction is got back in solvent tank within the condenser; Finally reduction vaporization precipitation is carried out to the Ovum Gallus domesticus Flavus lecithin in extraction kettle: in chuck and agitating vane, pass into steam heating and stir precipitation, stirring velocity 30 r/min, precipitation temperature controls at 50 DEG C, Ya Li – 0.09 below MPa to extraction kettle, the butane compression condensation liquefaction cycle of gasification uses; Finally obtain egg phospholipids mixture 1.1 kg, Oil of egg yolk 2.8 kg.
Collected Oil of egg yolk acid value is higher, need through depickling process, and first adopt massfraction to be that 95% ethanol carries out solvent extract deacidification, experiment condition is: Oil of egg yolk 2.8 kg, and ethanol contend 2.8 L, at room temperature extracts 120 min.With this understanding, the acid value of Oil of egg yolk is reduced to 19.4 mg KOH/g by 30.6 mg KOH/g.Adopt alkali-refining deacidification further afterwards, processing condition are: alkali lye mass concentration is 1%, and initial temperature is 20 DEG C, and final temperature is 50 DEG C, and the reaction times is 10 min.With this understanding, the acid value of Oil of egg yolk is reduced to 8.2 mgKOH/g by 19.4 mg KOH/g.
Carry out carrier preparation subsequently, adopt chemical coprecipitation: be dissolved in the 10 L aqueous solution by 9.3 g iron vitriols and 18 g Iron trichloride hexahydrates; Mechanical stirring revolution is 800 r/min; Then add 2.73 g PEG 6000, control temperature is 40 DEG C, deoxygenation 30 min; Afterwards under mechanical stirring state, add 25% ammonia soln fast, make the pH >10 of reaction soln, after stirring reaction 10 min, under vigorous stirring state, slowly add the CM-CTS that 1L concentration is 5%, after application of sample, temperature is elevated to rapidly 70 DEG C of reaction 30 min; After reaction terminates, under the effect of externally-applied magnetic field, sharp separation goes out magnetic-particle, by washed with de-ionized water for several times to remove unreacted chemical substance completely, until the pH of last solution is about 7; The magnetic carboxymethyl chitosan nano particle finally collecting black (is abbreviated as Fe
3o
4), and carry out lyophilize process (PEG+CM-CTS).Then Ca is adopted
2+to Fe
3o
4(PEG+CM-CTS) surface is modified further, processing condition are as follows: 1mg/mL Fe3O4 (PEG+CM-CTS) nano particle fully mixes with 2 mg/mL calcium chloride metal ion solutions, regulate the pH value of metal ion solution to 5.0, and under the Keep agitation state of 200 r/min, dynamic adsorption 30 min under the constant temperature of 25 DEG C, make it reach adsorption equilibrium, prepare Ca
2+the affine magnetic nanoparticle of immobilized metal modified, is abbreviated as Fe
3o
4(PEG+CM-CTS)@Ca
2+, finally the egg phospholipids obtained is adopted Fe further
3o
4(PEG+CM-CTS)@Ca (II) magnetic nanoparticle carries out separation and purification, and carry out desolventing technology (bleaching temperature 25 DEG C, application of sample amount 2.0%, bleaching time are 30 min) with neutral active charcoal, finally obtain high-purity PC 0.7 kg, high-purity PE 0.2 kg, PC purity >95%, PE purity >98%.
embodiment 2
By 100.0 kg Fresh Eggs, after picking egg, washing egg, through sterilization, (in the boiling water of 95 ~ 100 DEG C, immersion 5 ~ 7 is s), air-dry, is separated by egg white, obtains 28.0 kg egg yolk liquids after broken shell with egg white, yolk separating device with yolk.Add 28 L water in gained egg yolk liquid to dilute and after stirring, this yolk diluent is added in extractor, adding 504 L massfractions is subsequently 95 % ethanolic solns, at 80 KHz, lixiviate 5 times at 60 DEG C, each 60 min, recurrent interval 5 s, after extracting, vat liquor filters, filtrate discards precipitation in left at room temperature overnight and obtains yolk neutral fat vat liquor (including egg phospholipids), and paste is evaporated at 50 DEG C, recycling design, by the vacuum-drying at 65 DEG C of gained paste thing, obtain lurid Ovum Gallus domesticus Flavus lecithin crude extract 8.1 kg, collect alcohol-insoluble substance, reduction vaporization residual ethanol solvent, by pasteurize, spraying dry, cooling, sieve powder, obtains de-fatted egg yolk protein powder 4.7 kg.
8.1 kg Ovum Gallus domesticus Flavus lecithin crude extracts are placed in subcritical abstraction still, extraction kettle is vacuumized, utilize pressure difference to inject in extraction kettle by Propane in 48.6 L solvent tanks; Extraction process completes under complete totally enclosed processing condition, stirring velocity is 100 r/min, extraction temperature 60 DEG C, and pressure-controlling is at 1 Mpa, repeat lixiviate 5 times, each 10 min, after extraction terminates, mixing oil enters evaporating pot, under a reduced pressure, 70 DEG C of hot water heating precipitations, the propane of gasification is after compressor compression, and post liquefaction is got back in solvent tank within the condenser; Finally reduction vaporization precipitation is carried out to the Ovum Gallus domesticus Flavus lecithin in extraction kettle: in chuck and agitating vane, pass into steam heating and stir precipitation, stirring velocity 35 r/min, precipitation temperature controls at 70 DEG C, Ya Li below – 0.09MPa to extraction kettle, the propane compression condensation liquefaction of gasification recycles; Finally obtain egg phospholipids mixture 2.1 kg, Oil of egg yolk 5.8 kg.
Collected Oil of egg yolk acid value is higher, need through depickling process, and first adopt massfraction to be that 95% ethanol carries out solvent extract deacidification, experiment condition is: Oil of egg yolk 5.8 kg, ethanol contend 46.4 L, at room temperature extracts 5 times, each extraction 60 min.With this understanding, the acid value of Oil of egg yolk is reduced to 4.5mg KOH/g by 31.6 mg KOH/g.Adopt alkali-refining deacidification further afterwards, processing condition are: alkali lye mass concentration is 10%, and initial temperature is 60 DEG C, and final temperature is 65 DEG C, and the reaction times is 60 min.With this understanding, the acid value of Oil of egg yolk is reduced to 0.2 mg KOH/g by 4.5 mg KOH/g.
Carry out carrier preparation subsequently, adopt chemical coprecipitation: be dissolved in the 10L aqueous solution by 926.7 g aqueous ferrous sulfates and 450 g Iron trichloride hexahydrates; Mechanical stirring revolution is 200 r/min; Then add 137.67 g PEG 6000, control temperature is 70 DEG C, deoxygenation 30 min; Afterwards under mechanical stirring state, add 25% ammonia soln fast, make the pH >10 of reaction soln, after stirring reaction 10 min, under vigorous stirring state, slowly add the CM-CTS that 1L concentration is 5%, after application of sample, temperature is elevated to rapidly 90 DEG C of reaction 120 min; After reaction terminates, under the effect of externally-applied magnetic field, sharp separation goes out magnetic-particle, by washed with de-ionized water for several times to remove unreacted chemical substance completely, until the pH of last solution is about 7; The magnetic carboxymethyl chitosan nano particle finally collecting black (is abbreviated as Fe
3o
4), and carry out lyophilize process (PEG+CM-CTS).Then Ca is adopted
2+to Fe
3o
4(PEG+CM-CTS) surface is modified further, and processing condition are as follows: 1mg/mL Fe
3o
4(PEG+CM-CTS) nano particle fully mixes with 2 mg/mL calcium chloride metal ion solutions, regulate the pH value of metal ion solution to 8.0, and under the Keep agitation state of 800 r/min, dynamic adsorption 120 min under the constant temperature of 50 DEG C, make it reach adsorption equilibrium, prepare Ca
2+the affine magnetic nanoparticle of immobilized metal modified, is abbreviated as Fe
3o
4(PEG+CM-CTS)@Ca
2+; Finally the egg phospholipids obtained is adopted Fe further
3o
4(PEG+CM-CTS)@Ca (II) magnetic nanoparticle carries out separation and purification, and carry out desolventing technology (bleaching temperature 45 DEG C, application of sample amount 5.0%, bleaching time are for 90min) with neutral active charcoal, finally obtain high-purity PC 1.4 kg, high-purity PE 0.3 kg, PC purity>=95%, PE purity >95%.
embodiment 3
By 100.0 kg Fresh Eggs, after picking egg, washing egg, through sterilization, (in the boiling water of 95 ~ 100 DEG C, immersion 5 ~ 7 is s), air-dry, is separated by egg white, obtains 28.0 kg egg yolk liquids after broken shell with egg white, yolk separating device with yolk.Add 56 L water in gained egg yolk liquid to dilute and after stirring, this yolk diluent is added in ultrasonic extraction tank, add 126 L massfraction 90% ethanolic solns subsequently, at 40 KHz, lixiviate 2 times at 55 DEG C, each 30 min, recurrent interval 2 s, after extracting, vat liquor filters, filtrate discards precipitation in left at room temperature overnight and obtains yolk neutral fat vat liquor (including egg phospholipids), and paste is evaporated at 50 DEG C, recycling design, by the vacuum-drying at 55 DEG C of gained paste thing, obtain lurid Ovum Gallus domesticus Flavus lecithin crude extract 7.5 kg, collect alcohol-insoluble substance, reduction vaporization residual ethanol solvent, by pasteurize, spraying dry, cooling, sieve powder, obtains de-fatted egg yolk protein powder 5.3 kg.
7.5 kg Ovum Gallus domesticus Flavus lecithin crude extracts are placed in subcritical abstraction still, extraction kettle is vacuumized, utilize pressure difference to inject in extraction kettle by butane subcritical in 15 L solvent tanks; Extraction process completes under complete totally enclosed processing condition, stirring velocity is 80 r/min, extraction temperature 40 DEG C, and pressure-controlling is at 0.3 Mpa, repeat lixiviate 3 times, each 40 min, after extraction terminates, mixing oil enters evaporating pot, under a reduced pressure, 60 DEG C of hot water heating precipitations, the butane of gasification is after compressor compression, and post liquefaction is got back in solvent tank within the condenser; Finally reduction vaporization precipitation is carried out to the Ovum Gallus domesticus Flavus lecithin in extraction kettle: in chuck and agitating vane, pass into steam heating and stir precipitation, stirring velocity 60 r/min, precipitation temperature controls at 60 DEG C, Ya Li – 0.09 below MPa to extraction kettle, the butane compression condensation liquefaction cycle of gasification uses; Finally obtain egg phospholipids mixture 1.8 kg, Oil of egg yolk 5.4 kg.
Collected Oil of egg yolk acid value is higher, need through depickling process, and first adopt massfraction to be that 90% ethanol carries out solvent extract deacidification, experiment condition is: Oil of egg yolk 5.4 kg, ethanol contend 21.6 L, at room temperature extracts 4 times, each extraction 10 min.With this understanding, the acid value of Oil of egg yolk is reduced to 7.5 mg KOH/g by 31.6 mg KOH/g.Adopt alkali-refining deacidification further afterwards, processing condition are: alkali lye mass concentration is 8%, and initial temperature is 55 DEG C, and final temperature is 65 DEG C, and the reaction times is 30 min.With this understanding, the acid value of Oil of egg yolk is reduced to 0.1 mg KOH/g by 7.5 mg KOH/g.
Carry out carrier preparation subsequently, adopt chemical coprecipitation: 111.2g iron vitriol and 162g Iron trichloride hexahydrate are dissolved in the 10 L aqueous solution, mechanical stirring revolution is 800 r/min; Then add 27.3 g PEG 6000, control temperature is 60 DEG C, deoxygenation 30 min; Afterwards under mechanical stirring state, add sodium hydroxide solution fast, make the pH >10 of reaction soln, after stirring reaction 10 min, under vigorous stirring state, slowly add the CM-CTS that 1L concentration is 5%, after application of sample, temperature is elevated to rapidly 80 DEG C of reaction 60 min; After reaction terminates, under the effect of externally-applied magnetic field, sharp separation goes out magnetic-particle, by washed with de-ionized water for several times to remove unreacted chemical substance completely, until the pH of last solution is about 7; The magnetic carboxymethyl chitosan nano particle finally collecting black (is abbreviated as Fe
3o
4), and carry out lyophilize process (PEG+CM-CTS).Then Ca is adopted
2+to Fe
3o
4(PEG+CM-CTS) surface is modified further, and processing condition are as follows: 1mg/mL Fe
3o
4(PEG+CM-CTS) nano particle fully mixes with 2 mg/mL calcium chloride metal ion solutions, regulate the pH value of metal ion solution to 6.0, and under the Keep agitation state of 400 r/min, dynamic adsorption 90 min under the constant temperature of 37 DEG C, make it reach adsorption equilibrium, prepare Ca
2+the affine magnetic nanoparticle of immobilized metal modified, is abbreviated as Fe
3o
4(PEG+CM-CTS)@Ca
2+; Finally the egg phospholipids obtained is adopted Fe further
3o
4(PEG+CM-CTS)@Ca (II) magnetic nanoparticle carries out separation and purification, and carry out desolventing technology (bleaching temperature 35 DEG C, application of sample amount 4.0%, bleaching time are 60 min) with neutral active charcoal, finally obtain high-purity PC 1.2 kg, high-purity PE 0.2 kg, PC purity >95%, PE purity >97%.
Claims (2)
1. the co-production of Ovum Gallus domesticus Flavus lecithin, kephalin, Oil of egg yolk and low metaprotein powder, is characterized in that carrying out according to following step:
(1) yolk, egg white are separated:first to Fresh Egg inspection, cleaning and sterilization, after broken shell, yolk, egg white are separated, after yolk stirs, obtain fresh egg yolk liquid; The condition of sterilization is in the boiling water of 95 ~ 100 DEG C, soaks 5 ~ 7 s;
(2) extraction of neutral lipid:fresh egg yolk liquid and water are diluted by weight 1:1 ~ 1:3 and joins in ultrasonic extraction tank after stirring, and the massfraction adding 1 ~ 9 times of volume in extractor is 80 ~ 95% ethanolic solns, pulse ultrasonic wave is adopted to carry out assisted extraction subsequently, to extract mixture after 0.1 ~ 1 h through centrifugal or filtering separation, repeatedly extract 1 ~ 5 time, merge alcohol extract and be yolk neutral lipid extracting solution, wherein impulse ultrasound wave frequency 20 ~ 200 KHz, Extracting temperature 20 ~ 70 DEG C, extraction time 10 ~ 60 min, recurrent interval 1 ~ 5 s;
(3) concentrated, dry:the yolk neutral lipid extracting solution of step (2) gained is evaporated to paste, recycling design at 40 ~ 50 DEG C, by the vacuum-drying at 50 ~ 65 DEG C of gained paste thing, obtains light yellow egg phospholipids crude extract;
(4) preparation of de-fatted egg yolk protein powder:collect the alcohol-insoluble substance after massfraction is 80 ~ 95% extraction using alcohols in step (2), then 60 ~ 63 DEG C, 180 ~ 240 s carry out pasteurize, by spraying dry, drying conditions is inlet temperature 175 ~ 185 DEG C, air outlet temperature 75 ~ 80 DEG C, cools after powder delivery, through vibratory screening apparatus stage treatment;
(5) subcritical fluids is separated Oil of egg yolk:the Ovum Gallus domesticus Flavus lecithin crude extract that will obtain through step (3) loads extraction kettle, extraction kettle is vacuumized, utilize pressure difference Propane in solvent tank or subcritical butane to be injected in extraction kettle and carry out stirring-type countercurrent leaching, whole extraction process completes under complete totally enclosed processing condition; Wherein extraction conditions is: extracting times 1 ~ 5 time, solid-liquid ratio 1:1 ~ 1:6, extraction time 10 ~ 120 min, stirring velocity 35 ~ 100 r/min, extraction temperature 10 ~ 90 DEG C, pressure 0.2 ~ 1.0 Mpa; After extraction terminates, collect from extract and obtain Oil of egg yolk, from extract remainder, obtain de-oiling egg phospholipids mixture: PC and PE;
(6) egg phospholipids mixture precipitation:first steam or hot water is adopted to heat extractor, and stir, Heating temperature 10 ~ 110 DEG C, stirring velocity 30 ~ 100 r/min, still pressure to be extracted drops to 0.01MPa, enables vacuum pump and carries out negative pressure evaporation, until pressure is down to – 0.09 below MPa, open extractor, discharge low temperature de-oiling egg phospholipids mixture; Butane after gasification is compressed, after condensation liquefaction, get back in solvent tank and recycle;
(7) preparation of Oil of egg yolk:collect step (5) gained Oil of egg yolk, adopt massfraction to be 80 ~ 95% alcohol solvent extractions, then NaOH alkali refining method carries out depickling process to high acid value Oil of egg yolk crude product; Wherein, the parameter of alcohol solvent extraction method is: solid-liquid ratio: 1:1 ~ 1:8 (g:mL), extraction time 10 ~ 60 min, extraction times 1 ~ 5; The processing condition of NaOH alkali refining method are: alkali lye mass concentration is 1 ~ 10%, and initial temperature is 20 ~ 60 DEG C, and final temperature is 50 ~ 65 DEG C, and the reaction times is 10 ~ 60 min;
(8) preparation of magnetic Nano carrier of separating:adopt chemical coprecipitation: be dissolved in the aqueous solution by the iron vitriol of solubility and Iron trichloride hexahydrate, the two mol ratio is 1:2 ~ 2:1, and total iron concentration is 0.01 ~ 0.5 mol/L; Mechanical stirring revolution is 200 ~ 800 r/min; Then add polyethylene glycol 6000, its add-on is 1/10 of total weight of iron; Control temperature is 40 ~ 70 DEG C, deoxygenation 30 min; Afterwards under mechanical stirring state, add 25% ammoniacal liquor or sodium hydroxide alkaline solution fast, make the pH >10 of reaction soln, under vigorous stirring state, the carboxymethyl chitosan solution that mass concentration is 5 % is slowly added after stirring reaction 10 min, the add-on of carboxymethyl chitosan solution is 1/10 of total reaction liquor capacity, after application of sample, temperature is elevated to rapidly 70 ~ 90 DEG C of reaction 30 ~ 120 min; After reaction terminates, under the effect of externally-applied magnetic field, sharp separation goes out magnetic-particle, by washed with de-ionized water for several times to remove unreacted chemical substance completely, until the pH of last solution is about 7; Finally collect the magnetic carboxymethyl chitosan nano particle of black, and carry out lyophilize process; Then Ca is adopted
2+modify further magnetic carboxymethyl chitosan nano grain surface, processing condition are as follows: the magnetic carboxymethyl chitosan nano particle of 1 mg/mL respectively with the Ca of 2 mg/mL
2+solution mixes, and regulate the pH value of mixing solutions to 5.0 ~ 8.0, and under the Keep agitation state of 200 ~ 800 r/min, dynamic adsorption 30 ~ 120 min, makes it reach adsorption equilibrium, prepare Ca under the constant temperature of 25 ~ 50 DEG C
2+the affine magnetic nanoparticle of immobilized metal modified, wherein provides Ca
2+be the combination of a kind of in calcium chloride, calcium carbonate, calcium phosphate, caoxalate, calcium acetate or two kinds;
(9) separation and purification of PC, PE:employing massfraction is the precipitation egg phospholipids mixture of 80 ~ 95% dissolve with ethanol solution step (6) gained, adds Ca afterwards
2+the affine magnetic nanoparticle of immobilized metal modified, at 0 ~ 37 DEG C of stirring reaction 10 ~ 180 min, makes the PE in phospholipid complex solution specifically be adsorbed on Ca
2+the immobilized metal modified is affine, and magnetic nanoparticle is surperficial, under the effect of externally-applied magnetic field, the magnetic nanoparticle being adsorbed with PE is separated from reaction soln, as eluent, wash-out is carried out to its magnetic carrier using any one in EDTA-2Na or 1 ~ 25% ammonia soln, collect elutriant, dialysis, concentrated, prepare high-purity PE; Carrier, after wash-out, can utilize Ca
2+solution regenerates, and realizes the recycling of magnetic carrier;
(10) decolouring of yolk PC:collect the adsorption liquid after step (9) process, and adopt the process of neutral active carbon decoloring, bleaching temperature 25 ~ 45 DEG C, discoloring agent addition 2.0 ~ 5.0%, bleaching time are 30 ~ 90 min.
2. the co-production of Ovum Gallus domesticus Flavus lecithin according to claim 1, kephalin, Oil of egg yolk and low metaprotein powder, is characterized in that impulse ultrasound wave frequency 20 ~ 80 KHz in step (2); Extracting temperature 45 ~ 60 DEG C; Extraction time 10 ~ 60 min, extraction temperature 40-60 DEG C in step (5).
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| DE19828799A1 (en) * | 1998-06-27 | 1999-12-30 | Meyer Lucas Gmbh & Co | Fractionation of lecithin by alcohol extraction to obtain extract with increased phosphatidylcholine content |
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