CN101019599A - Combined prepn process of wheat plumule protein and its derivative product - Google Patents
Combined prepn process of wheat plumule protein and its derivative product Download PDFInfo
- Publication number
- CN101019599A CN101019599A CNA2007100782564A CN200710078256A CN101019599A CN 101019599 A CN101019599 A CN 101019599A CN A2007100782564 A CNA2007100782564 A CN A2007100782564A CN 200710078256 A CN200710078256 A CN 200710078256A CN 101019599 A CN101019599 A CN 101019599A
- Authority
- CN
- China
- Prior art keywords
- filtrate
- wheat
- filter residue
- vacuum
- filter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The present invention relates to the preparation process of wheat plumule products, and is especially the combined preparation process of wheat plumule protein and other derivative products. By using dried wheat plumule as main material and through defatting, solvent extracting, separating, enzyme hydrolyzing and other technological steps, the present invention prepares alcohol wheat plumule protein as well as antioxidant and antisenility wheat plumule liquid, hydrolyzed wheat plumule peptide concentrate, hydrolyzed wheat plumule peptide powder, wheat plumule protein feed additive and other products. The preparation process has the decolorize and solvent reused. The preparation process has best utilization of wheat plumule resource, advanced operation, low cost and other advantages, and the products may be used widely and has great marketability.
Description
One. technical field
The invention belongs to agricultural byproducts wheat embryo evaluation and exploration technology field, particularly the preparation method of wheat embryo product.
Two. background technology
Wheat is to plant cereal crops the most widely in the world, and it is main food with the wheat flour that the whole world has 35～40% population approximately, and the wheat of China is second important crops that is only second to paddy rice.The affluent resources that the wheat amount of being is many, wide.Make full use of wheat resource, very important meaning is arranged.
The main application of wheat is to be processed into wheat flour for human edible, and wheat embryo is the accessory substance in the wheat flour process.Wheat embryo accounts for about 3% of wheat seed, contains the composition that 15～40% good protein, 10～20% grease and dietary fibre, mineral matter, vitamin etc. are of value to health in the plumule, is described as " human natural nutrition storehouse " by the nutritionist.Wheat embryo is widely used in various nutriment, health products, the remedy diet abroad.Alcohol soluble protein in the wheat plantule protein is one of preparation drug coating, medicinal slow release agent, shampoo slipping agent, food fresh keeping primary raw material of filming etc., also is used to prepare anti-oxidation peptide, high F value oligopeptide, step-down peptide and fat substitute etc.Wheat embryo peptide and wheat embryo are anti-oxidant, anti-senility liquid contains multiple little molecule small peptide, amino acid, vitamin and mineral elements such as glutathione, nutritive value is high, can be used for the nutrition renovation agent that health products, food and daily use chemicals industry are cooked nutrition fortifier and anti-ageing, antifatigue, antioxidant, hair, skin etc.Therefore, develop the wheat embryo resource in recent years, become the research focus of industries such as domestic and international food, biochemistry, nutrition.
The method of existing development and use wheat embryo resource, as the patent No. is " a kind of hydrolysate of wheat plantule protein and preparation method and purposes " patent of ZL03158292.3, the wheat embryo that discloses with degreasing is a raw material, the wheat gluten hydrolysate of preparing, it only is a kind of mixture of polypeptide compounds, wheat embryo alcohol soluble protein and wheat embryo polyphenoils are not separated, are underused the wheat embryo resource yet..The patent No. " wheat plantule protein beverage " patent of ZL03126118.3 not and for example discloses this beverage and has mainly contained 5～25% wheat embryo, emulsifing thickener, fumet, antioxidant, sweetener, makes the aqueous solution.This patent has just directly been utilized a spot of wheat embryo resource, do not remove the grease in the wheat embryo, from wheat embryo, do not prepare the wheat plantule protein product, its resource utilization is low, owing to contain the grease of very easily oxidation in the beverage, easily oxidation, become sour, influence product stability and taste.
Three. summary of the invention
The objective of the invention is weak point at existing development and use wheat embryo resource method, the combined preparation process of a kind of wheat plantule protein and derived product thereof is provided, can prepare simultaneously that wheat embryo alcohol soluble protein, hydrolyzed wheat plumule peptide concentrate, wheat-germ oil, wheat embryo are anti-oxidant, anti-senility liquid, the multiple wheat embryo product of hydrolyzed wheat germ flour agent feedstuff additive, and have the wheat embryo of making full use of resource, technology is simple, preparation cost is cheap, is convenient to characteristics such as industrial production.
Principle of the present invention: utilize wheat embryo to be raw material, extract wherein embryo oil, obtain the wheat embryo crude oil and the defatted wheat germ dregs of rice with benzinum or n-hexane degreasing agent; Small peptides such as glutathione in the defatted wheat germ dregs of rice, amino acid and pure alcohol soluble protein all are dissolvable in water in 50%～80% the ethanolic solution, therefore, the ethanolic solution of available this scope extracts, and obtains extract, under reduced pressure, reclaim ethanol, obtain concentrate.After removing ethanol, wheat gliadin is separated out, and through separate dissolved, obtains wheat gliadin liquid or convection drying and becomes the wheat gliadin powder; Solution after the extraction wheat embryo alcohol soluble protein is made small peptides such as containing glutathione and anti-oxidant, the anti-senility liquid of amino acid whose wheat embryo by decolouring, ultrafiltration and concentrated the allotment; With extract, preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, the residue of anti-senility liquid, carry out enzyme associating hydrolysis, through going out enzyme, liquid, slag separate again, decolouring concentrates, spray-drying obtains hydrolyzed wheat plumule peptide.This product also has anti-oxidant, anti-senescence function except that having trophism.
The object of the present invention is achieved like this: the combined preparation process of a kind of wheat plantule protein and derived product thereof is a raw material with the drying wheat plumule, obtains through technologies such as degreasing, solvent extraction, separation, enzyme hydrolysis.The concrete grammar step of preparing the wheat embryo multiple product is as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent n-hexane or benzinum is 1: 3～5 ratio, drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, refluxing extraction is carried out in the degreasing 5～6 hours that refluxes under 50～70 ℃ of temperature altogether 3～6 times.After each extraction is finished, filter, and collect filtrate and filter residue respectively.Its filtrate is the wheat embryo crude oil, and filter residue is the defatted wheat germ dregs of rice.
2. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining, prepare refining wheat embryo oil product.
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure and handles except that degreasing agent, remove degreasing agent after, just prepare the defatted wheat germ dregs of rice.
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 50～80% ethanolic solution is 1: 10～20 ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1～1.5 hour, and stirred altogether and extract 2～5 times.After each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively.Filter residue is used to prepare hydrolyzed wheat plumule peptide, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
2. concentrating and separating
Filtrate to (2)-1. step collected is positioned in the decompressor, carries out reduced vacuum and concentrates, be-0.06 in vacuum～-0.08Mpa, thickening temperature is that the concentration that is concentrated into soluble solid is 25～35% under 75～90 ℃ the condition.Vacuum places separator with concentrate after concentrating and finishing, and takes out after cooling off 10～16 hours under 0～4 ℃ of temperature, filters with 100～160 purpose nylon screens, and collects filter residue and filtrate respectively.Its filter residue is the wheat embryo alcoholic solution albumen crude product that solidifies, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
3. decolouring separates
Filtrate to the collection of (2)-2. step, weight according to decolorizer such as HZ-802, HZ-803 polymeric adsorbent or ROHM AND HAAS polymeric adsorbent (Amberlite XAD-6HP) etc.: the volume ratio of filtrate is 1: 10～20 ratio, in filtrate, add decolorizer, stirring decolours handled 10～30 minutes, filter then, collect filtrate and filter residue respectively.Its filter residue is the decolorizer filter residue, can reuse after the regeneration.The concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 20～25%, once more in the solution after regulating solubility solid concentration, add the solvent propane diols of this liquor capacity 5～15% or the anticorrisive agent sorbic acid of glycerine and this liquor capacity 0.02～0.05%, after stirring, filter with diatomite earlier, remove impurity, be that 0.22～0.5 micron miillpore filter carries out vacuum filtration with the aperture again, vacuum is-0.06～-0.08Mpa, further remove impurity, collect filtrate, just preparing total glutathione content is 0.2～1%, a-amino acid content is 10～15%, the pH value is that 5～6 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product.
4. washing separates
To the wheat embryo alcohol soluble protein crude product filter residue that solidifies that (2)-2. step collected,, and collect filter residue and filtrate with a spot of 0～4 ℃ distilled water flushing, filtration.To the filter residue of collecting, be positioned in the vacuum tank, add glycerine of 6～8 times of its solid weights and the solvent propane diols of 3～1 times of its solid weights, be warming up to 60～70 ℃, be-0.06 in vacuum～-condition of 0.08Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 7～10% wheat embryo alcohol soluble protein liquid product.Filtrate to collecting is used to prepare hydrolyzed wheat plumule peptide.
5. regenerate decolorizer and solvent
With the decolorizer filter residue that (2)-3. step collected, add the subacidity methyl alcohol or the alcohol solvent of 4～8 times of its weight, under agitation handled 30～90 minutes, filter then, collect filtrate and filter residue respectively.Filtrate to collecting is positioned in the vacuum tank, is warming up to 60～90 ℃, be-0.06 in vacuum～-distill condensation process under the condition of 0.08Mpa, collection solvent methanol or ethanol distillation condensate liquid, recycling.To the filter residue of collecting, be neutrality with distilled water cyclic washing to pH value till, collect the decolorizer filter residue of regenerating, can be used to once more prepare that wheat embryo is anti-oxidant, the decolouring of anti-senility liquid processing.
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 10～15 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 1～3 hour, under agitation be warming up to 50～65 ℃, be incubated after 30～60 minutes, the neutral proteinase that adds filter residue weight 0.5～2%, insulation hydrolysis 1～2 hour, the flavor protease that adds filter residue weight 0.2～0.5% again, continue hydrolysis 1～3 hour, regulating its pH value with watery hydrochloric acid then is 4.8～5.2, just prepares the wheat embryo peptide hydrolysate.
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 3000～5000r/min centrifugal 10～20 minutes, collect centrifugation and clear liquid respectively.To the precipitation of collecting, distilled water with 4～6 times of its weight disperses earlier, be that 135～165 ℃, leaving air temp are that 85～95 ℃, spraying centrifuge speed are under the condition of 6000～8000r/min at EAT again, carry out spray-drying, just prepare the wheat plantule protein feedstuff additive product.
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, adds the wood activated charcoal of its volume 3～5%, is warming up to 85～95 ℃, stirs decolouring 15～30min, carries out vacuum filtration then, collects filter residue and filtrate respectively.To the filter residue of collecting, send active carbon recovery plant to regenerate after, recycling.
4. vacuum concentrates
The filtrate that (3)-3. step was collected, vacuum-0.06～-0.08MPa, temperature carry out reduced vacuum under 75～85 ℃ the condition to concentrate, and reaches 20～25% until its soluble solid concentration, just prepares hydrolyzed wheat plumule peptide concentrate.
5. allotment, secondary filter
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the propane diols of concentrate volume 5～15% and the sorbic acid of concentrate volume 0.05～0.08% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carry out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again, just prepare the hydrolyzed wheat plumule peptide concentrate product that is used for cosmetics.
Perhaps go on foot the hydrolyzed wheat plumule peptide concentrate of preparing with (3)-4., at EAT is that 135～155 ℃, leaving air temp are that 75～85 ℃, spraying centrifuge speed are under the condition of 8000～10000r/min, carry out spray-drying, just prepare powdery hydrolyzed wheat plumule peptide product.This product both can be used for food, can be used for health products again.
After the present invention adopts technique scheme, mainly contain following characteristics:
1. fully utilize the wheat embryo resource.The present invention is raw material with the wheat embryo, can prepare simultaneously that wheat embryo alcohol soluble protein, wheat embryo are anti-oxidant, anti-senility liquid, hydrolyzed wheat plumule peptide concentrate, used for cosmetic hydrolyzed wheat plumule concentrate, hydrolyzed wheat plumule peptide powder and wheat plantule protein feed addictive multiple product, the wheat processing byproduct wheat embryo resource that the amount of making full use of is many, wide is for DEVELOPMENT AND UTILIZATION OF WHEAT GERM provides new way.
2. the inventive method in process of production; can be to decolorizer, wood activated charcoal and ethanol or the equal reproducible utilization of methanol solvate that uses; this had both made full use of physical resources, had reduced production costs; avoid the discharging of industrial pollutants again; help environmental protection, belong to the friendly process preparation method that nothing " three wastes " is polluted.
3. the production technology advanced person of the inventive method, Standardization instrument, easy and simple to handle, with low cost, easy to utilize.
The wheat embryo product that adopts the present invention to prepare can be widely used in industries such as food, biochemistry, pharmacy, daily use chemicals, nutrient and healthcare products, feed processing, and range of application is wide, and the market competitiveness is strong.
Four. the specific embodiment
Below in conjunction with the specific embodiment, further specify the present invention
Embodiment 1
The concrete steps of the combined preparation process of a kind of wheat plantule protein and derived product thereof are as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent n-hexane is 1: 3 a ratio, and drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, and refluxing extraction is carried out in the degreasing 5 hours that refluxes under 50 ℃ of temperature altogether 3 times.After each extraction is finished, filter, and collect filtrate and filter residue respectively.Its filtrate is the wheat embryo crude oil, and filter residue is the defatted wheat germ dregs of rice.
2. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining, prepare refining wheat embryo oil product.
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure and handles except that degreasing agent, remove degreasing agent after, just prepare the defatted wheat germ dregs of rice.
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 50% ethanolic solution is 1: 10 a ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1 hour, stir altogether and extract 2 times.After each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively.Filter residue is used to prepare hydrolyzed wheat plumule peptide, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
2. concentrating and separating
Filtrate to (2)-1. step collected is positioned in the decompressor, carries out reduced vacuum and concentrates, and in vacuum is-0.06Mpa, and thickening temperature is that the concentration that is concentrated into soluble solid is 25% under 75 ℃ the condition.Vacuum places separator with concentrate after concentrating and finishing, and takes out after 10 hours in cooling under 0 ℃ of temperature, filters with 100 purpose nylon screens, and collects filter residue and filtrate respectively.Its filter residue is the wheat embryo alcoholic solution albumen crude product that solidifies, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
3. decolouring separates
The filtrate that (2)-2. step was collected, according to the weight of decolorizer HZ-802: the volume ratio of filtrate is 1: 10 a ratio, adds decolorizer in filtrate, and stirring decolours handled 10 minutes, filtered then, collected filtrate and filter residue respectively.Its filter residue is the decolorizer filter residue, can reuse after the regeneration.The concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 20%, once more in the solution after regulating solubility solid concentration, add the solvent propane diols of this liquor capacity 5% and the anticorrisive agent sorbic acid of this liquor capacity 0.02%, after stirring, filter with diatomite earlier, remove impurity, be that 0.22 micron miillpore filter carries out vacuum filtration with the aperture again, vacuum is-0.06Mpa, further remove impurity, collect filtrate, just preparing total glutathione content is 0.2%, a-amino acid content is 10%, the pH value is that 5 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product.
4. washing separates
To the wheat embryo alcohol soluble protein crude product filter residue that solidifies that (2)-2. step collected,, and collect filter residue and filtrate with a spot of 0 ℃ distilled water flushing, filtration.To the filter residue of collecting, be positioned in the vacuum tank, add glycerine of 6 times of its solid weights and the solvent propane diols of 3 times of its solid weights, be warming up to 60 ℃, in vacuum be-condition of 0.06Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 7% wheat embryo alcohol soluble protein liquid product.Filtrate to collecting is used to prepare hydrolyzed wheat plumule peptide.
5. regenerate decolorizer and solvent
With the decolorizer filter residue that (2)-3. step collected, add the subacidity methanol solvate of 4 times of its weight, under agitation handled 30 minutes, filter then, collect filtrate and filter residue respectively.Filtrate to collecting is positioned in the vacuum tank, is warming up to 60 ℃, distills condensation process under the condition of vacuum for-0.06Mpa, collects solvent methanol distillation condensate liquid, and is recycling.To the filter residue of collecting, be neutrality with distilled water cyclic washing to pH value till, collect the decolorizer filter residue of regenerating, can be used to once more prepare that wheat embryo is anti-oxidant, the decolouring of anti-senility liquid processing.
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 10 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 1 hour, under agitation be warming up to 50 ℃, be incubated after 30 minutes, the neutral proteinase that adds filter residue weight 0.5%, insulation hydrolysis 1 hour, the flavor protease that adds filter residue weight 0.2% again, continue hydrolysis 1 hour, regulating its pH value with watery hydrochloric acid then is 4.8, just prepares the wheat embryo peptide hydrolysate.
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 3000r/min centrifugal 10 minutes, collect centrifugation and clear liquid respectively.To the precipitation of collecting, disperse earlier with the distilled water of 4 times of its weight, be that 135 ℃, leaving air temp are 85 ℃, the centrifuge speed of spraying is under the condition of 6000r/min at EAT again, carry out spray-drying, just prepare the wheat plantule protein feedstuff additive product.
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, adds the wood activated charcoal of its volume 3%, is warming up to 85 ℃, stirs decolouring 15min, carries out vacuum filtration then, collects filter residue and filtrate respectively.To the filter residue of collecting, send active carbon recovery plant to regenerate after, recycling.
4. vacuum concentrates
The filtrate that (3)-3. step was collected is to carry out reduced vacuum under 75 ℃ the condition to concentrate in vacuum-0.06MPa, temperature, reaches 20% until its soluble solid concentration, just prepares hydrolyzed wheat plumule peptide concentrate.
5. allotment, secondary filter
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the glycerine of concentrate volume 5% and the sorbic acid of concentrate volume 0.05% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carry out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again, just prepare the hydrolyzed wheat plumule peptide concentrate product that is used for cosmetics.
Perhaps go on foot the hydrolyzed wheat plumule peptide concentrate of preparing with (3)-4., at EAT is that 135 ℃, leaving air temp are that 75 ℃, spraying centrifuge speed are under the condition of 8000r/min, carry out spray-drying, just prepare powdery hydrolyzed wheat plumule peptide product.This product both can be used for food, can be used for health products again.
Embodiment 2
The concrete steps of the combined preparation process of a kind of wheat plantule protein and derived product thereof are as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent n-hexane is 1: 5 a ratio, and drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, and refluxing extraction is carried out in the degreasing 6 hours that refluxes under 70 ℃ of temperature altogether 6 times.After each extraction is finished, filter, and collect filtrate and filter residue respectively.Its filtrate is the wheat embryo crude oil, and filter residue is the defatted wheat germ dregs of rice.
2. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining, prepare refining wheat embryo oil product.
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure and handles except that degreasing agent, remove degreasing agent after, just prepare the defatted wheat germ dregs of rice.
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 80% ethanolic solution is 1: 20 a ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1.5 hours, stir altogether and extract 5 times.After each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively.Filter residue is used to prepare hydrolyzed wheat plumule peptide, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
2. concentrating and separating
Filtrate to (2)-1. step collected is positioned in the decompressor, carries out reduced vacuum and concentrates, and in vacuum is-0.08Mpa, and thickening temperature is that the concentration that is concentrated into soluble solid is 35% under 90 ℃ the condition.Vacuum places separator with concentrate after concentrating and finishing, and takes out after 16 hours in cooling under 4 ℃ of temperature, filters with 160 purpose nylon screens, and collects filter residue and filtrate respectively.Its filter residue is the wheat embryo alcoholic solution albumen crude product that solidifies, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
3. decolouring separates
The filtrate that (2)-2. step was collected, according to the weight of decolorizer HZ-803 polymeric adsorbent: the volume ratio of filtrate is 1: 20 a ratio, adds decolorizer in filtrate, and stirring decolours handled 30 minutes, filtered then, collected filtrate and filter residue respectively.Its filter residue is the decolorizer filter residue, can reuse after the regeneration.The concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 25%, once more in the solution after regulating solubility solid concentration, add the solvent glycerin of this liquor capacity 15% and the anticorrisive agent sorbic acid of this liquor capacity 0.05%, after stirring, filter with diatomite earlier, remove impurity, be that 0.5 micron miillpore filter carries out vacuum filtration with the aperture again, vacuum is-0.08Mpa, further remove impurity, collect filtrate, just preparing total glutathione content is 1%, a-amino acid content is 15%, the pH value is that 6 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product.
4. washing separates
To the wheat embryo alcohol soluble protein crude product filter residue that solidifies that (2)-2. step collected,, and collect filter residue and filtrate with a spot of 4 ℃ distilled water flushing, filtration.To the filter residue of collecting, be positioned in the vacuum tank, add glycerine of 8 times of its solid weights and the solvent propane diols of 1 times of its solid weight, be warming up to 70 ℃, in vacuum be-condition of 0.08Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 10% wheat embryo alcohol soluble protein liquid product.Filtrate to collecting is used to prepare hydrolyzed wheat plumule peptide.
5. regenerate decolorizer and solvent
With the decolorizer filter residue that (2)-3. step collected, add the subacidity alcohol solvent of 8 times of its weight, under agitation handled 90 minutes, filter then, collect filtrate and filter residue respectively.Filtrate to collecting is positioned in the vacuum tank, is warming up to 90 ℃, distills condensation process under the condition of vacuum for-0.08Mpa, collects etoh solvent distillation condensate liquid, and is recycling.To the filter residue of collecting, be neutrality with distilled water cyclic washing to pH value till, collect the decolorizer filter residue of regenerating, can be used to once more prepare that wheat embryo is anti-oxidant, the decolouring of anti-senility liquid processing.
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 15 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 3 hours, under agitation be warming up to 65 ℃, be incubated after 60 minutes, the neutral proteinase that adds filter residue weight 2%, insulation hydrolysis 2 hours, the flavor protease that adds filter residue weight 0.5% again, continue hydrolysis 3 hours, regulating its pH value with watery hydrochloric acid then is 5.2, just prepares the wheat embryo peptide hydrolysate.
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 5000r/min centrifugal 20 minutes, collect centrifugation and clear liquid respectively.To the precipitation of collecting, disperse earlier with the distilled water of 6 times of its weight, be that 165 ℃, leaving air temp are 95 ℃, the centrifuge speed of spraying is under the condition of 8000r/min at EAT again, carry out spray-drying, just prepare the wheat plantule protein feedstuff additive product.
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, adds the wood activated charcoal of its volume 5%, is warming up to 95 ℃, stirs decolouring 30min, carries out vacuum filtration then, collects filter residue and filtrate respectively.To the filter residue of collecting, send active carbon recovery plant to regenerate after, recycling.
4. vacuum concentrates
The filtrate that (3)-3. step was collected is to carry out reduced vacuum under 85 ℃ the condition to concentrate in vacuum-0.08MPa, temperature, reaches 25% until its soluble solid concentration, just prepares hydrolyzed wheat plumule peptide concentrate.
5. allotment, secondary filter
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the propane diols of concentrate volume 15% and the sorbic acid of concentrate volume 0.08% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carry out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again, just prepare the hydrolyzed wheat plumule peptide concentrate product that is used for cosmetics.
Perhaps go on foot the hydrolyzed wheat plumule peptide concentrate of preparing with (3)-4., at EAT is that 155 ℃, leaving air temp are that 85 ℃, spraying centrifuge speed are under the condition of 10000r/min, carry out spray-drying, just prepare powdery hydrolyzed wheat plumule peptide product.This product both can be used for food, can be used for health products again.
Embodiment 3
The concrete steps of the combined preparation process of a kind of wheat plantule protein and derived product thereof are as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent benzinum is 1: 4 a ratio, and drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, and refluxing extraction is carried out in the degreasing 5.5 hours that refluxes under 60 ℃ of temperature altogether 5 times.After each extraction is finished, filter, and collect filtrate and filter residue respectively.Its filtrate is the wheat embryo crude oil, and filter residue is the defatted wheat germ dregs of rice.
3. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining, prepare refining wheat embryo oil product.
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure and handles except that degreasing agent, remove degreasing agent after, just prepare the defatted wheat germ dregs of rice.
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 70% ethanolic solution is 1: 15 a ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1.3 hours, stir altogether and extract 3 times.After each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively.Filter residue is used to prepare hydrolyzed wheat plumule peptide, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
2. concentrating and separating
Filtrate to (2)-1. step collected is positioned in the decompressor, carries out reduced vacuum and concentrates, and in vacuum is-0.07MPa, and thickening temperature is that the concentration that is concentrated into soluble solid is 30% under 80 ℃ the condition.Vacuum places separator with concentrate after concentrating and finishing, and takes out after 13 hours in cooling under 3 ℃ of temperature, filters with 120 purpose nylon screens, and collects filter residue and filtrate respectively.Its filter residue is the wheat embryo alcoholic solution albumen crude product that solidifies, and filtrate being used to prepares anti-oxidant, the anti-senility liquid of wheat embryo.
3. decolouring separates
Filtrate to the collection of (2)-2. step, weight according to decolorizer ROHM AND HAAS polymeric adsorbent (Amberlite XAD-6HP): the volume ratio of filtrate is 1: 15 a ratio, adds decolorizer in filtrate, and stirring decolours handled 20 minutes, filter then, collect filtrate and filter residue respectively.Its filter residue is the decolorizer filter residue, can reuse after the regeneration.The concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 23%, once more in the solution after regulating solubility solid concentration, add the solvent glycerin of this liquor capacity 10% and the anticorrisive agent sorbic acid of this liquor capacity 0.3%, after stirring, filter with diatomite earlier, remove impurity, be that 0.4 micron miillpore filter carries out vacuum filtration with the aperture again, vacuum is-0.07 Mpa, further remove impurity, collect filtrate, just preparing total glutathione content is 0.5%, a-amino acid content is 13%, the pH value is that 5.6 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product.
4. washing separates
To the wheat embryo alcohol soluble protein crude product filter residue that solidifies that (2)-2. step collected,, and collect filter residue and filtrate with a spot of 2 ℃ distilled water flushing, filtration.To the filter residue of collecting, be positioned in the vacuum tank, add glycerine of 7 times of its solid weights and the solvent propane diols of 2 times of its solid weights, be warming up to 65 ℃, in vacuum be-condition of 0.07Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 8% wheat embryo alcohol soluble protein liquid product.Filtrate to collecting is used to prepare hydrolyzed wheat plumule peptide.
5. regenerate decolorizer and solvent
With the decolorizer filter residue that (2)-3. step collected, add the subacidity methanol solvate of 6 times of its weight, under agitation handled 60 minutes, filter then, collect filtrate and filter residue respectively.Filtrate to collecting is positioned in the vacuum tank, is warming up to 80 ℃, distills condensation process under the condition of vacuum for-0.07Mpa, collects solvent methanol distillation condensate liquid, and is recycling.To the filter residue of collecting, be neutrality with distilled water cyclic washing to pH value till, collect the decolorizer filter residue of regenerating, can be used to once more prepare that wheat embryo is anti-oxidant, the decolouring of anti-senility liquid processing.
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 13 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 2 hours, under agitation be warming up to 55 ℃, be incubated after 45 minutes, the neutral proteinase that adds filter residue weight 1%, insulation hydrolysis 1.5 hours, the flavor protease that adds filter residue weight 0.35% again, continue hydrolysis 2 hours, regulating its pH value with watery hydrochloric acid then is 5.0, just prepares the wheat embryo peptide hydrolysate.
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 4000r/min centrifugal 15 minutes, collect centrifugation and clear liquid respectively.To the precipitation of collecting, disperse earlier with the distilled water of 5 times of its weight, be that 155 ℃, leaving air temp are 90 ℃, the centrifuge speed of spraying is under the condition of 7000r/min at EAT again, carry out spray-drying, just prepare the wheat plantule protein feedstuff additive product.
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, adds the wood activated charcoal of its volume 4%, is warming up to 90 ℃, stirs decolouring 20min, carries out vacuum filtration then, collects filter residue and filtrate respectively.To the filter residue of collecting, send active carbon recovery plant to regenerate after, recycling.
4. vacuum concentrates
The filtrate that (3)-3. step was collected is to carry out reduced vacuum under 80 ℃ the condition to concentrate in vacuum-0.07MPa, temperature, reaches 23% until its soluble solid concentration, just prepares hydrolyzed wheat plumule peptide concentrate.
5. allotment, secondary filter
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the propane diols of concentrate volume 10% and the sorbic acid of concentrate volume 0.06% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carry out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again, just prepare the hydrolyzed wheat plumule peptide concentrate product that is used for cosmetics.
Perhaps go on foot the hydrolyzed wheat plumule peptide concentrate of preparing with (3)-4., at EAT is that 150 ℃, leaving air temp are that 80 ℃, spraying centrifuge speed are under the condition of 9000r/min, carry out spray-drying, just prepare powdery hydrolyzed wheat plumule peptide product.This product both can be used for food, can be used for health products again.
Claims (4)
1. the combined preparation process of wheat plantule protein and derived product thereof is characterized in that concrete method step is as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent n-hexane or benzinum is 1: 3～5 ratio, drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, degreasing 5～6 hours refluxes under 50～70 ℃ of temperature, carry out refluxing extraction altogether 3～6 times, after each extraction is finished, filter, and collect filtrate and filter residue respectively;
2. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining;
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure except that the degreasing agent processing;
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 50～80% ethanolic solution is 1: 10～20 ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1～1.5 hour, stir altogether and extract 2～5 times, after each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively;
2. concentrating and separating
Filtrate to the collection of (2)-1. step, be positioned in the decompressor, carry out reduced vacuum and concentrate, be-0.06 in vacuum～-0.08Mpa, thickening temperature is under 75～90 ℃ the condition, the concentration that is concentrated into soluble solid is 25～35%, vacuum places separator with concentrate after concentrating and finishing, and takes out after cooling off 10～16 hours under 0～4 ℃ of temperature, filter with 100～160 purpose nylon screens, and collect filter residue and filtrate respectively;
3. decolouring separates
Filtrate to the collection of (2)-2. step, according to decolorizer such as HZ-802, the weight of HZ-803 polymeric adsorbent or ROHM AND HAAS polymeric adsorbent: the volume ratio of filtrate is 1: 10～20 ratio, in filtrate, add decolorizer, stirring decolours handled 10～30 minutes, filter then, collect filtrate and filter residue respectively, the concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 20～25%, once more in the solution after regulating solubility solid concentration, add the solvent propane diols of this liquor capacity 5～15% or the anticorrisive agent sorbic acid of glycerine and this liquor capacity 0.02～0.05%, after stirring, filter with diatomite earlier, be that 0.22～0.5 micron miillpore filter carries out vacuum filtration with the aperture again, vacuum is-0.06～-0.08Mpa, collect filtrate, just preparing total glutathione content is 0.2～1%, a-amino acid content is 10～15%, the pH value is that 5～6 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product;
4. washing separates
The wheat embryo alcohol soluble protein crude product filter residue that solidifies to the collection of (2)-2. step, with a spot of 0～4 ℃ distilled water flushing, filtration, and collection filter residue and filtrate, to the filter residue of collecting, be positioned in the vacuum tank, add glycerine of 6～8 times of its solid weights and the solvent propane diols of 3～1 times of its solid weights, be warming up to 60～70 ℃, be-0.06 in vacuum～-condition of 0.08Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 7～10% wheat embryo alcohol soluble protein liquid product;
5. regenerate decolorizer and solvent
Decolorizer filter residue with the collection of (2)-3. step, the subacidity methyl alcohol or the alcohol solvent that add 4～8 times of its weight, under agitation handled 30～90 minutes, filter then, collect filtrate and filter residue respectively, to the filtrate of collecting, be positioned in the vacuum tank, be warming up to 60～90 ℃, be-0.06 in vacuum～-distill condensation process under the condition of 0.08Mpa, collect solvent methanol or ethanol distillation condensate liquid, to the filter residue of collecting, till being neutrality with distilled water cyclic washing to pH value, collect regeneration decolorizer filter residue;
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 10～15 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 1～3 hour, under agitation be warming up to 50～65 ℃, be incubated after 30～60 minutes, the neutral proteinase that adds filter residue weight 0.5～2%, insulation hydrolysis 1～2 hour, the flavor protease that adds filter residue weight 0.2～0.5% again, continue hydrolysis 1～3 hour, regulating its pH value with watery hydrochloric acid then is 4.8～5.2;
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 3000～5000r/min centrifugal 10～20 minutes, collect centrifugation and clear liquid respectively, to the precipitation of collecting, distilled water with 4～6 times of its weight disperses earlier, be that 135～165 ℃, leaving air temp are that 85～95 ℃, spraying centrifuge speed are under the condition of 6000～8000r/min at EAT again, carry out spray-drying;
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, the wood activated charcoal that adds its volume 3～5%, be warming up to 85～95 ℃, stir decolouring 15～30min, carry out vacuum filtration then, collect filter residue and filtrate respectively, filter residue to collecting send active carbon recovery plant to regenerate;
4. vacuum concentrates
The filtrate that (3)-3. step was collected, vacuum-0.06～-0.08MPa, temperature carry out reduced vacuum under 75～85 ℃ the condition to concentrate, and reaches 20～25% until its soluble solid concentration;
5. allotment, secondary filter
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the propane diols of concentrate volume 5～15% and the sorbic acid of concentrate volume 0.05～0.08% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carries out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again;
Perhaps with (3)-4. hydrolyzed wheat plumule peptide concentrate prepared of step, be that 135～155 ℃, leaving air temp are that 75～85 ℃, spraying centrifuge speed are under the condition of 8000～10000r/min at EAT, carry out spray-drying.
2. according to the combined preparation process of described wheat plantule protein of claim 1. and derived product thereof, it is characterized in that the concrete steps of combined preparation process of a kind of wheat plantule protein and derived product thereof are as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent n-hexane is 1: 3 a ratio, drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, degreasing 5 hours refluxes under 50 ℃ of temperature, carry out refluxing extraction altogether 3 times, after each extraction is finished, filter, and collect filtrate and filter residue respectively;
2. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining;
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure except that the degreasing agent processing;
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 50% ethanolic solution is 1: 10 a ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1 hour, stir altogether and extract 2 times, after each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively;
2. concentrating and separating
Filtrate to the collection of (2)-1. step, be positioned in the decompressor, carry out reduced vacuum and concentrate, in vacuum be-0.06Mpa, thickening temperature is under 75 ℃ the condition, the concentration that is concentrated into soluble solid is 25%, vacuum places separator with concentrate after concentrating and finishing, and takes out after 10 hours in cooling under 0 ℃ of temperature, filter with 100 purpose nylon screens, and collect filter residue and filtrate respectively;
3. decolouring separates
Filtrate to the collection of (2)-2. step, weight according to decolorizer HZ-802: the volume ratio of filtrate is 1: 10 a ratio, in filtrate, add decolorizer, stirring decolours handled 10 minutes, filter then, collect filtrate and filter residue respectively, the concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 20%, once more in the solution after regulating solubility solid concentration, add the solvent propane diols of this liquor capacity 5% and the anticorrisive agent sorbic acid of this liquor capacity 0.02%, after stirring, filtering with diatomite earlier, is that 0.22 micron miillpore filter carries out vacuum filtration with the aperture again, and vacuum is-0.06Mpa, collect filtrate, just preparing total glutathione content is 0.2%, a-amino acid content is 10%, the pH value is that 5 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product;
4. washing separates
The wheat embryo alcohol soluble protein crude product filter residue that solidifies to the collection of (2)-2. step, with a spot of 0 ℃ distilled water flushing, filtration, and collection filter residue and filtrate, filter residue to collecting is positioned in the vacuum tank, adds glycerine of 6 times of its solid weights and the solvent propane diols of 3 times of its solid weights, be warming up to 60 ℃, in vacuum be-condition of 0.06Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 7% wheat embryo alcohol soluble protein liquid product;
5. regenerate decolorizer and solvent
With the decolorizer filter residue that (2)-3. step collected, add the subacidity methanol solvate of 4 times of its weight, under agitation handled 30 minutes, filter then, collect filtrate and filter residue respectively, the filtrate to collecting is positioned in the vacuum tank, be warming up to 60 ℃, under the condition of vacuum, distill condensation process, collect solvent methanol distillation condensate liquid, the filter residue of collecting for-0.06Mpa, till being neutrality with distilled water cyclic washing to pH value, collect regeneration decolorizer filter residue;
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 10 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 1 hour, under agitation be warming up to 50 ℃, be incubated after 30 minutes, the neutral proteinase that adds filter residue weight 0.5%, insulation hydrolysis 1 hour, the flavor protease that adds filter residue weight 0.2% again, continue hydrolysis 1 hour, regulating its pH value with watery hydrochloric acid then is 4.8;
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 3000r/min centrifugal 10 minutes, collect centrifugation and clear liquid respectively, to the precipitation of collecting, distilled water with 4 times of its weight disperses earlier, be that 135 ℃, leaving air temp are that 85 ℃, spraying centrifuge speed are under the condition of 6000r/min at EAT again, carry out spray-drying;
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, adds the wood activated charcoal of its volume 3%, be warming up to 85 ℃, stir decolouring 15min, carry out vacuum filtration then, collect filter residue and filtrate respectively, the filter residue to collecting send active carbon recovery plant to regenerate;
4. vacuum concentrates
The filtrate that (3)-3. step was collected is to carry out reduced vacuum under 75 ℃ the condition to concentrate in vacuum-0.06MPa, temperature, reaches 20% until its soluble solid concentration;
5. allotment, secondary filter
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the glycerine of concentrate volume 5% and the sorbic acid of concentrate volume 0.05% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carries out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again;
Perhaps with (3)-4. hydrolyzed wheat plumule peptide concentrate prepared of step, be that 135 ℃, leaving air temp are that 75 ℃, spraying centrifuge speed are under the condition of 8000r/min at EAT, carry out spray-drying.
3. according to the combined preparation process of described wheat plantule protein of claim 1. and derived product thereof, it is characterized in that the concrete steps of combined preparation process of a kind of wheat plantule protein and derived product thereof are as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent n-hexane is 1: 5 a ratio, drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, degreasing 6 hours refluxes under 70 ℃ of temperature, carry out refluxing extraction altogether 6 times, after each extraction is finished, filter, and collect filtrate and filter residue respectively;
2. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining;
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure except that the degreasing agent processing;
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 80% ethanolic solution is 1: 20 a ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1.5 hours, stir altogether and extract 5 times, after each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively;
2. concentrating and separating
Filtrate to the collection of (2)-1. step, be positioned in the decompressor, carry out reduced vacuum and concentrate, in vacuum be-0.08Mpa, thickening temperature is under 90 ℃ the condition, the concentration that is concentrated into soluble solid is 35%, vacuum places separator with concentrate after concentrating and finishing, and takes out after 16 hours in cooling under 4 ℃ of temperature, filter with 160 purpose nylon screens, and collect filter residue and filtrate respectively;
3. decolouring separates
Filtrate to the collection of (2)-2. step, weight according to decolorizer HZ-803 polymeric adsorbent: the volume ratio of filtrate is 1: 20 a ratio, in filtrate, add decolorizer, stirring decolours handled 30 minutes, filter then, collect filtrate and filter residue respectively, the concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 25%, once more in the solution after regulating solubility solid concentration, add the solvent glycerin of this liquor capacity 15% and the anticorrisive agent sorbic acid of this liquor capacity 0.05%, after stirring, filter with diatomite earlier, be that 0.5 micron miillpore filter carries out vacuum filtration with the aperture again, vacuum is-0.08Mpa, collect filtrate, just preparing total glutathione content is 1%, a-amino acid content is 15%, the pH value is that 6 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product;
4. washing separates
The wheat embryo alcohol soluble protein crude product filter residue that solidifies to the collection of (2)-2. step, with a spot of 4 ℃ distilled water flushing, filtration, and collection filter residue and filtrate, filter residue to collecting is positioned in the vacuum tank, adds glycerine of 8 times of its solid weights and the solvent propane diols of 1 times of its solid weight, be warming up to 70 ℃, in vacuum be-condition of 0.08Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 10% wheat embryo alcohol soluble protein liquid product;
5. regenerate decolorizer and solvent
With the decolorizer filter residue that (2)-3. step collected, add the subacidity alcohol solvent of 8 times of its weight, under agitation handled 90 minutes, filter then, collect filtrate and filter residue respectively, the filtrate to collecting is positioned in the vacuum tank, be warming up to 90 ℃, under the condition of vacuum, distill condensation process, collect etoh solvent distillation condensate liquid, the filter residue of collecting for-0.08Mpa, till being neutrality with distilled water cyclic washing to pH value, collect regeneration decolorizer filter residue;
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 15 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 3 hours, under agitation be warming up to 65 ℃, be incubated after 60 minutes, the neutral proteinase that adds filter residue weight 2%, insulation hydrolysis 2 hours, the flavor protease that adds filter residue weight 0.5% again, continue hydrolysis 3 hours, regulating its pH value with watery hydrochloric acid then is 5.2;
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 5000r/min centrifugal 20 minutes, collect centrifugation and clear liquid respectively, to the precipitation of collecting, distilled water with 6 times of its weight disperses earlier, be that 165 ℃, leaving air temp are that 95 ℃, spraying centrifuge speed are under the condition of 8000r/min at EAT again, carry out spray-drying;
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, adds the wood activated charcoal of its volume 5%, be warming up to 95 ℃, stir decolouring 30min, carry out vacuum filtration then, collect filter residue and filtrate respectively, the filter residue to collecting send active carbon recovery plant to regenerate;
4. vacuum concentrates
The filtrate that (3)-3. step was collected is to carry out reduced vacuum under 85 ℃ the condition to concentrate in vacuum-0.08MPa, temperature, reaches 25% until its soluble solid concentration;
5. allotment, secondary filter
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the propane diols of concentrate volume 15% and the sorbic acid of concentrate volume 0.08% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carries out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again;
Perhaps with (3)-4. hydrolyzed wheat plumule peptide concentrate prepared of step, be that 155 ℃, leaving air temp are that 85 ℃, spraying centrifuge speed are under the condition of 10000r/min at EAT, carry out spray-drying.
4. according to the combined preparation process of described wheat plantule protein of claim 1. and derived product thereof, it is characterized in that the concrete steps of combined preparation process of a kind of wheat plantule protein and derived product thereof are as follows:
(1) the preparation wheat-germ oil and the defatted wheat germ dregs of rice
1. degreasing refluxes
Weight in the drying wheat plumule: the volume ratio of degreasing agent benzinum is 1: 4 a ratio, drying wheat plumule and degreasing agent are positioned in the refluxing extraction device, degreasing 5.5 hours refluxes under 60 ℃ of temperature, carry out refluxing extraction altogether 5 times, after each extraction is finished, filter, and collect filtrate and filter residue respectively;
2. handle filtrate and filter residue
To the wheat embryo crude oil filtrate that (1)-1. step collected, adopt existing wheat-germ oil method of refining to carry out refining;
Defatted wheat germ dregs of rice filter residue with (1)-1. step collected places Desolventizing apparatus, adopts existing wheat embryo dregs of rice Desolventizing method to reduce pressure except that the degreasing agent processing;
(2) preparation wheat embryo alcohol soluble protein and wheat embryo is anti-oxidant, anti-senility liquid
1. ethanol dissolving
(1) step finish after, weight in the defatted wheat germ dregs of rice prepared in (1)-2. step: concentration is that the volume ratio of 70% ethanolic solution is 1: 15 a ratio, the defatted wheat germ dregs of rice and ethanolic solution are positioned in the container, stirred at normal temperatures 1.3 hours, stir altogether and extract 3 times, after each extraction is finished, carry out vacuum filtration, and collect filtrate and filter residue respectively;
2. concentrating and separating
Filtrate to the collection of (2)-1. step, be positioned in the decompressor, carry out reduced vacuum and concentrate, in vacuum be-0.07MPa, thickening temperature is under 80 ℃ the condition, the concentration that is concentrated into soluble solid is 30%, vacuum places separator with concentrate after concentrating and finishing, and takes out after 13 hours in cooling under 3 ℃ of temperature, filter with 120 purpose nylon screens, and collect filter residue and filtrate respectively;
3. decolouring separates
Filtrate to the collection of (2)-2. step, weight according to decolorizer ROHM AND HAAS polymeric adsorbent: the volume ratio of filtrate is 1: 15 a ratio, in filtrate, add decolorizer, stirring decolours handled 20 minutes, filter then, collect filtrate and filter residue respectively, the concentration that the filtrate of collecting is regulated its solubility solid with distilled water is 23%, once more in the solution after regulating solubility solid concentration, add the solvent glycerin of this liquor capacity 10% and the anticorrisive agent sorbic acid of this liquor capacity 0.3%, after stirring, filter with diatomite earlier, be that 0.4 micron miillpore filter carries out vacuum filtration with the aperture again, vacuum is-0.07Mpa, collect filtrate, just preparing total glutathione content is 0.5%, a-amino acid content is 13%, the pH value is that 5.6 light yellow transparent wheat embryo is anti-oxidant, the anti-senility liquid product;
4. washing separates
The wheat embryo alcohol soluble protein crude product filter residue that solidifies to the collection of (2)-2. step, with a spot of 2 ℃ distilled water flushing, filtration, and collection filter residue and filtrate, filter residue to collecting is positioned in the vacuum tank, adds glycerine of 7 times of its solid weights and the solvent propane diols of 2 times of its solid weights, be warming up to 65 ℃, in vacuum be-condition of 0.07Mpa under, carry out transpiring moisture and handle to solution transparently, just prepare protein concentration and be 8% wheat embryo alcohol soluble protein liquid product;
5. regenerate decolorizer and solvent
With the decolorizer filter residue that (2)-3. step collected, add the subacidity methanol solvate of 6 times of its weight, under agitation handled 60 minutes, filter then, collect filtrate and filter residue respectively, the filtrate to collecting is positioned in the vacuum tank, be warming up to 80 ℃, under the condition of vacuum, distill condensation process, collect solvent methanol distillation condensate liquid, the filter residue of collecting for-0.07Mpa, till being neutrality with distilled water cyclic washing to pH value, collect regeneration decolorizer filter residue;
(3) preparation wheat embryo peptide concentrate and powder
1. hydrolysis
The filter residue of collecting in (2)-1. step that is used for preparing hydrolyzed wheat plumule peptide, the filtrate that is used to prepare hydrolyzed wheat plumule peptide that adds the collection of (2)-4. step earlier, the distilled water that adds 13 times of filter residue weight again, soak and be placed in the hydrolysis kettle in 2 hours, under agitation be warming up to 55 ℃, be incubated after 45 minutes, the neutral proteinase that adds filter residue weight 1%, insulation hydrolysis 1.5 hours, the flavor protease that adds filter residue weight 0.35% again, continue hydrolysis 2 hours, regulating its pH value with watery hydrochloric acid then is 5.0;
2. centrifugation
The wheat embryo peptide hydrolysate of (3)-1. step preparation is placed centrifuge, with the rotating speed of 4000r/min centrifugal 15 minutes, collect centrifugation and clear liquid respectively, to the precipitation of collecting, distilled water with 5 times of its weight disperses earlier, be that 155 ℃, leaving air temp are that 90 ℃, spraying centrifuge speed are under the condition of 7000r/min at EAT again, carry out spray-drying;
3. decolouring
The centrifugal clear liquid that (3)-2. step was collected places the decolouring still, under agitation, adds the wood activated charcoal of its volume 4%, be warming up to 90 ℃, stir decolouring 20min, carry out vacuum filtration then, collect filter residue and filtrate respectively, the filter residue to collecting send active carbon recovery plant to regenerate;
4. vacuum concentrates
The filtrate that (3)-3. step was collected is to carry out reduced vacuum under 80 ℃ the condition to concentrate in vacuum-0.07MPa, temperature, reaches 23% until its soluble solid concentration;
5. allotment, secondary filter:
Go on foot in the wheat embryo peptide concentrate of preparing (3)-4., adding the propane diols of concentrate volume 10% and the sorbic acid of concentrate volume 0.06% allocates, after stirring, miillpore filter with 0.5 μ m filters earlier, carries out aseptic filtration and sterile filling with 0.22 μ m miillpore filter again;
Perhaps with (3)-4. hydrolyzed wheat plumule peptide concentrate prepared of step, be that 150 ℃, leaving air temp are that 80 ℃, spraying centrifuge speed are under the condition of 9000r/min at EAT, carry out spray-drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100782564A CN100553470C (en) | 2007-03-05 | 2007-03-05 | The combined preparation process of wheat plantule protein and derived product thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100782564A CN100553470C (en) | 2007-03-05 | 2007-03-05 | The combined preparation process of wheat plantule protein and derived product thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101019599A true CN101019599A (en) | 2007-08-22 |
| CN100553470C CN100553470C (en) | 2009-10-28 |
Family
ID=38707531
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100782564A Expired - Fee Related CN100553470C (en) | 2007-03-05 | 2007-03-05 | The combined preparation process of wheat plantule protein and derived product thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100553470C (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212598A (en) * | 2011-04-02 | 2011-10-12 | 重庆大学 | Method for preparing quaternary ammonium hydrolysis wheat peptide concentrated solution from gluten |
| CN102326687A (en) * | 2011-07-14 | 2012-01-25 | 山东六和集团有限公司 | Broiler compound feed with wheat germs and preparation method thereof |
| CN102342555A (en) * | 2011-01-28 | 2012-02-08 | 王宇飞 | Wheat germ-sesame protein fermented beverage and preparation process thereof |
| CN102406049A (en) * | 2011-10-25 | 2012-04-11 | 江苏江大源生态生物科技有限公司 | Joint preparation method of wheat germ oil and wheat germ protein |
| CN102504936A (en) * | 2011-10-24 | 2012-06-20 | 陈元涛 | Process for preparing barley germ oil and low molecular weight peptide by solid enzymolysis-CO2 (carbon dioxide) supercritical extraction |
| CN103039717A (en) * | 2013-01-23 | 2013-04-17 | 江南大学 | Preparation technology of polypeptide feed additive containing wheat or wheat processing products |
| CN103555689A (en) * | 2013-11-15 | 2014-02-05 | 长沙理工大学 | Comprehensive utilization method of wheat germination product |
| CN103875906A (en) * | 2014-03-03 | 2014-06-25 | 中国科学院过程工程研究所 | Comprehensive wheat germ meal utilization method |
| CN104543327A (en) * | 2014-12-29 | 2015-04-29 | 徐州绿之野生物食品有限公司 | Preparation method of gingko prolamin |
| CN104642715A (en) * | 2015-03-10 | 2015-05-27 | 安徽天利粮油集团股份有限公司 | Method for extracting rice germ protein |
| CN105385732A (en) * | 2015-11-16 | 2016-03-09 | 中国农业科学院农产品加工研究所 | Method for efficiently preparing vital gluten short peptides through double-enzyme composite enzymatic hydrolysis |
| CN109463538A (en) * | 2018-12-28 | 2019-03-15 | 河北肽都生物科技有限公司 | A kind of preparation method of milk cow small molecule feed peptide |
| CN109576331A (en) * | 2018-12-21 | 2019-04-05 | 河北肽都生物科技有限公司 | A kind of extracting method of wheat germ peptide |
-
2007
- 2007-03-05 CN CNB2007100782564A patent/CN100553470C/en not_active Expired - Fee Related
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102342555A (en) * | 2011-01-28 | 2012-02-08 | 王宇飞 | Wheat germ-sesame protein fermented beverage and preparation process thereof |
| CN102212598A (en) * | 2011-04-02 | 2011-10-12 | 重庆大学 | Method for preparing quaternary ammonium hydrolysis wheat peptide concentrated solution from gluten |
| CN102212598B (en) * | 2011-04-02 | 2013-08-07 | 重庆大学 | Method for preparing quaternary ammonium hydrolysis wheat peptide concentrated solution from gluten |
| CN102326687A (en) * | 2011-07-14 | 2012-01-25 | 山东六和集团有限公司 | Broiler compound feed with wheat germs and preparation method thereof |
| CN102504936A (en) * | 2011-10-24 | 2012-06-20 | 陈元涛 | Process for preparing barley germ oil and low molecular weight peptide by solid enzymolysis-CO2 (carbon dioxide) supercritical extraction |
| CN102504936B (en) * | 2011-10-24 | 2013-08-28 | 陈元涛 | Process for preparing barley germ oil and low molecular weight peptide by solid enzymolysis-CO2 (carbon dioxide) supercritical extraction |
| CN102406049A (en) * | 2011-10-25 | 2012-04-11 | 江苏江大源生态生物科技有限公司 | Joint preparation method of wheat germ oil and wheat germ protein |
| CN103039717A (en) * | 2013-01-23 | 2013-04-17 | 江南大学 | Preparation technology of polypeptide feed additive containing wheat or wheat processing products |
| CN103555689A (en) * | 2013-11-15 | 2014-02-05 | 长沙理工大学 | Comprehensive utilization method of wheat germination product |
| CN103555689B (en) * | 2013-11-15 | 2015-11-25 | 长沙理工大学 | A kind of method of comprehensive utilization of wheat germination product |
| CN103875906A (en) * | 2014-03-03 | 2014-06-25 | 中国科学院过程工程研究所 | Comprehensive wheat germ meal utilization method |
| CN103875906B (en) * | 2014-03-03 | 2015-11-04 | 中国科学院过程工程研究所 | A kind of method of comprehensive utilization of the wheat embryo dregs of rice |
| CN104543327A (en) * | 2014-12-29 | 2015-04-29 | 徐州绿之野生物食品有限公司 | Preparation method of gingko prolamin |
| CN104642715A (en) * | 2015-03-10 | 2015-05-27 | 安徽天利粮油集团股份有限公司 | Method for extracting rice germ protein |
| CN105385732A (en) * | 2015-11-16 | 2016-03-09 | 中国农业科学院农产品加工研究所 | Method for efficiently preparing vital gluten short peptides through double-enzyme composite enzymatic hydrolysis |
| CN105385732B (en) * | 2015-11-16 | 2018-11-06 | 中国农业科学院农产品加工研究所 | A kind of method that double-enzyme composite hydrolysis prepares Gluten small peptide |
| CN109576331A (en) * | 2018-12-21 | 2019-04-05 | 河北肽都生物科技有限公司 | A kind of extracting method of wheat germ peptide |
| CN109463538A (en) * | 2018-12-28 | 2019-03-15 | 河北肽都生物科技有限公司 | A kind of preparation method of milk cow small molecule feed peptide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100553470C (en) | 2009-10-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100553470C (en) | The combined preparation process of wheat plantule protein and derived product thereof | |
| CN103843970B (en) | Production method for preparing ossein oligopeptide meal, bone oil and bone meal | |
| US20050106300A1 (en) | Method for producing a material having an increased solubility in alcohol | |
| CN101880596A (en) | Method for preparing oil at low temperature | |
| CN100465285C (en) | Method for extracting carnosine | |
| CN101288437B (en) | Method for producing soy protein peptides and dietary fiber from defated soybean pulp | |
| CN101015336A (en) | Prepn. of coconut extractive | |
| CN103014108A (en) | Preparation method of corn oligopeptide | |
| CN105949290A (en) | Chickpea protein powder and oligo-peptide powder and preparation methods and uses thereof | |
| CN103478838A (en) | Honeysuckle kudzuvine root beverage and preparation method thereof | |
| CN105238551A (en) | Method for supercritical CO2 extraction and purification of camellia seed oil | |
| CN104286856A (en) | Production method of odorless high-purity soybean oligopeptide | |
| Türker et al. | Waste (water) to feed protein: Effluent characteristics, protein recovery, and single-cell protein production from food industry waste streams | |
| CN107385003A (en) | A kind of preparation technology of soy peptide powder | |
| CN104262453A (en) | Gradient extraction method for plant protein | |
| CN108159283A (en) | The extracting method and purposes of the compound free amino acid of stem of noble dendrobium blade | |
| US6602985B1 (en) | Extraction of zein protein from gluten meal | |
| US6228993B1 (en) | Soy isoflavone concentrate process and product | |
| CN102652556B (en) | Preparation method of instant kudzuvine root particles | |
| CN108530553A (en) | A kind of preparation method of chick-pea neutral polysaccharide | |
| CN100415697C (en) | Agent of extracting polyphenol from rape seed cakes or husks and its preparation | |
| CN101289394A (en) | Process for abstracting chlorogenic acid and separating protein and small peptide form sunflower meal | |
| EP2038388B1 (en) | Process for aqueous oil extraction from oilseed starting material | |
| CN107459547A (en) | The coproduction separation method of various bioactivators in yolk | |
| CN102952002A (en) | Method for refining magnolol through supersonic extraction separating technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Zhengda Kangdi (Chenghai) Co. Ltd. Assignor: Chongqing University Contract record no.: 2010440000759 Denomination of invention: Combined prepn process of wheat plumule protein and its derivative product Granted publication date: 20091028 License type: Exclusive License Open date: 20070822 Record date: 20100612 |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091028 Termination date: 20100305 |