CN104095141B - A kind of method of chicken bone coproduction collagen active peptide and flavor base material - Google Patents
A kind of method of chicken bone coproduction collagen active peptide and flavor base material Download PDFInfo
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Abstract
The present invention discloses a kind of method of chicken bone coproduction collagen active peptide and flavor base material, by adopting two sections of hot pressing method for extracting, and through slight pressure release ftercompction process, increases substantially the product rate extracting collagen active peptide from chicken bone; By the ossein in extract was carried out high-pressure homogeneous before carrying out stepwise discretization reaction, it is to increase the degree of hydrolysis of enzymolysis solution. In addition, by enzymolysis solution is carried out two-stage ultrafiltration, realize the separation and purification of different product in enzymolysis solution, and carry out following process for each point of subsegment product and obtain comprising the variant productions such as the bone polysaccharide of chondroitin sulfate, macromole polypeptide and micromolecule polypeptide, realize making full use of ossein enzymolysis solution, carry out Maillard reaction especially by by macromole polypeptide and wood sugar, halfcystine and VitB1, obtain flavor base material with rich flavor.
Description
Technical field
The present invention relates to biological technical field, particularly relate to a kind of method of chicken bone coproduction collagen active peptide and flavor base material.
Background technology
In Jin10Nian Lai world meat production, chicken output increases very fast, and China's chicken output occupies second place of the world, and chicken bone annual production up to 7,000,000 tons, can account for the 25% of livestock and poultry gross weight alive. Chicken osteotrophy is quite abundant, and its protein is similar with the fresh meat of lipid content and equivalent, is respectively 16.3% and 14.5%, and the mineral elements such as calcium, phosphorus, iron and zinc are the several times of fresh meat, and ratio is suitable for, and wherein calcium contents is 3.95%, and phosphorus content is 2.04%. Chicken bone protein is the soluble protein of comparatively full price, biological value height, is the protein source of high-quality. In addition, chicken bone also contains the nutrient substance of other needed by human a large amount of, such as each seed amino acid and vitamin A, D, B1��B12Deng, especially contain the indispensable phospholipid of brain and phosphorprotein, old and feeble and that strengthen tegumental cell metabolism osso-albumin and chondroitin sulfate can be prevented, and the egg ammonia enzyme of liver function can be promoted. As can be seen here, chicken bone has important comprehensive utilization and Development volue, but for a long time due to the reason of the aspect such as fund, technology, a large amount of chicken bones is not reasonably utilized, and it is processed to the product that added value is very low, such as bone mud, feed or fertilizer etc., it does not have embody the nutritive value of chicken bone completely, the abandoned that even has also causes serious environmental pollution. Along with the development of China's bird processing industry, how to realize chicken bone higher value application, it is to increase the added value that utilizes of chicken bone is the severe problem faced at present.
At present, the collagen protein in chicken bone or chondroitin sulfate are mainly extracted in the utilization of chicken bone, although the processing method adopted can extract the II collagen type in chicken bone cartilage, but the extraction yield of the I-type collagen in the os osseum accounting for skeleton quality about 60% is very low or be only that chicken bone enzymolysis is obtained chondroitin sulfate, enzymolysis solution is then as wastewater treatment, the utilization ratio of these methods not only chicken bone is low, environment also causes bigger pollution simultaneously.
Summary of the invention
It is an object of the invention to provide a kind of method of chicken bone coproduction collagen active peptide and flavor base material, by adopting two sections of hot pressing method for extracting, and process through slight pressure release ftercompction, chicken bone is made to obtain abundant pyrolysis, I-type collagen in os osseum and the II collagen type etc. in cartilage are fully extracted, thus increase substantially the product rate extracting collagen active peptide from chicken bone;In addition, by the ossein in extract was carried out high-pressure homogeneous before carrying out stepwise discretization reaction, promote that in ossein, collagen protein carries out physics depolymerization, thus increase substantially the degree of hydrolysis of enzymolysis solution.
Another object of the present invention is, by the ossein in extract is carried out stepwise discretization by compound protease and flavor protease, compound protease can increase restriction enzyme site on the one hand, thus increase the effect of enzymolysis, obtain a large amount of polypeptide, peptide molecule chain end is modified by flavor protease on the other hand, it is to increase the product local flavor of collagen active peptide.
Another object of the present invention is, by enzymolysis solution is carried out two-stage ultrafiltration, realize the separation and purification of different product in enzymolysis solution, and carry out following process for each point of subsegment product and obtain comprising the variant productions such as the bone polysaccharide of chondroitin sulfate, macromole polypeptide and micromolecule polypeptide, realize making full use of ossein enzymolysis solution, carry out Maillard reaction especially by by macromole polypeptide and wood sugar, halfcystine and VitB1, obtain flavor base material with rich flavor.
The technical scheme of the present invention is:
A kind of method of chicken bone coproduction collagen active peptide and flavor base material, it is characterised in that,
Chicken bone is carried out two sections of hot pressing extractings and obtains extract, and carry out stepwise discretization after the ossein extracted from extract is carried out high-pressure homogeneous process, wherein said two sections of hot pressing method for extracting are: mixed according to 1: 1-2 mass ratio with water by chicken bone, carry out one section of hot pressing extracting and two sections of hot pressing extractings in turn, wherein one section of hot pressing extraction temperature is 110-120 DEG C, extracting time 100-120min, two sections of hot pressing extraction temperatures are 130-140 DEG C, extracting time 70-90min;
In addition, also comprise the following steps:
Step one, stepwise discretization react, and are mixed with compound protease and flavor protease respectively according to sequencing by the ossein after high-pressure homogeneous process and carry out stepwise discretization reaction, obtain enzymolysis solution;
Step 2, two-stage ultrafiltering, the ultra-filtration membrane that gained enzymolysis solution employing molecular weight cut-off is 9-10kDa is carried out one-level ultrafiltration, obtain one-level and retain liquid and one-level filtrate, the ultra-filtration membrane that one-level filtrate employing molecular weight cut-off is 2-3kDa is carried out two-stage ultrafiltering, obtains second entrapment liquid and two grades of filtrates;
The preparation of step 3, flavor base material, gained one-level retains liquid adopts ethanol precipitation to process, leave standstill precipitation, get supernatant liquor and second entrapment liquid is mixed to form Maillard reaction precursor, hot pressure reaction is carried out after being mixed with a certain amount of wood sugar, halfcystine and VitB1 by gained Maillard reaction precursor, obtain maillard reaction product, by after gained maillard reaction product concentrate drying both described flavor base material;
The two grades of filtrates of gained in step 2 are carried out concentrate drying and had both obtained collagen active peptide by the preparation of step 4, collagen active peptide.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, described two sections of hot pressing extractive reactions carry out in hot pressure reaction tank, and after two sections of hot pressing extractive reactions terminate, carry out slight pressure release ftercompction, concrete grammar is: after two sections of hot pressing extractings terminate, and opens the pressure release valve 8-10min of hot pressure reaction tank, makes to close after decrease in temperature 5-10 DEG C in hot pressure reaction tank pressure release valve 8-10min, and make rise in temperature 5-10 DEG C, repeat 3-5 time according to this step.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, in step one, the quality of added compound protease and flavor protease is respectively the 0.2-0.3% of ossein quality used, enzyme digestion reaction temperature is 51-53 DEG C, each step enzyme digestion reaction carries out 100-120min respectively, and each step enzyme digestion reaction is warming up to 90-100 DEG C respectively and keeps 20-30min to carry out enzyme-deactivating after terminating.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, the concrete grammar of ethanol precipitation described in step 3 is: described one-level retained after liquid mixes according to the volume ratio of 1: 2-3 with 90-100% ethanol, centrifugal through 8000-10000r/min, obtain supernatant and lower sediment.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, after ethanol precipitation gained lower sediment is processed 2-3 time with 90-100% ethanol dehydration, obtain chondroitin sulfate after drying.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, in step 3, the quality of added wood sugar, halfcystine and VitB1 is respectively the 0.4-0.6% of Maillard reaction precursor mass used, described hot pressure reaction temperature is 100-110 DEG C, and the hot pressure reaction time is 80-100min.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, the extracting method of described ossein is: carry out stratification after gained extract screens out bone slag, remove after upper oil phase both described ossein;
In addition, ossein is carried out high-pressure homogeneous method is: adopt high pressure homogenizer to carry out high-pressure homogeneous to ossein, wherein sets homogenizing temperature 70 �� 2 DEG C, pressure 30 �� 2MPa, rotating speed 700-800r/min, homogenizing time 5-8min.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, adopting vibratory screening apparatus division to carry out bone slag and screen out, vibratory screening apparatus aperture used is 40-50 order, and can through pulverizing, drying is prepared as bone meal by remaining bone slag in the bone slag that screens out and hot pressure reaction tank.
Preferably, in described chicken bone coproduction collagen active peptide and the method for flavor base material, get the upper oil phase after stratification and upper oil phase is heated to about 80 DEG C, add the 90-95 DEG C of hot water that volume is upper oil phase 10-15%, 10-15r/min stirs 8-10min, remove aqueous phase after standing sedimentation 20-30min, surplus oil heat phase is obtained animal oil to being cooled to 80-85 DEG C within 30min after 100-115 DEG C.
The present invention has following useful effect: the method for a kind of chicken bone coproduction collagen active peptide of the present invention and flavor base material, by adopting two sections of hot pressing method for extracting, and process through slight pressure release ftercompction, chicken bone is made to obtain abundant pyrolysis, the collagen proteins such as the I-type collagen in os osseum and the II collagen type in cartilage are fully extracted, the content of collagen protein in extract is made to reach about 40mg/g, especially for the extraction of the I-type collagen in os osseum, traditional atmospheric cooking method is difficult to the I-type collagen extracting in os osseum, and I-type collagen extraction yield in os osseum is improve more than 3 times by the present invention, I-type collagen in os osseum is utilized effectively, and increase substantially the product rate extracting collagen active peptide from chicken bone, the content of peptides of products therefrom reaches 91%, in addition, by the ossein in extract was carried out high-pressure homogeneous before carrying out stepwise discretization reaction, promote that in ossein, collagen protein carries out physics depolymerization, thus increase substantially the degree of hydrolysis of enzymolysis solution, degree of hydrolysis is made to reach more than 30%, and traditional method degree of hydrolysis only can reach about 20%.
In addition, by the ossein in extract is carried out stepwise discretization by compound protease and flavor protease, compound protease can increase restriction enzyme site on the one hand, can the abundant enzymolysis not easily former albumen of dissolved gum, thus increase the effect of enzymolysis, obtain a large amount of polypeptide, peptide molecule chain end is modified by flavor protease on the other hand, the bitter peptides content that enzymolysis is produced is controlled, and fresh taste peptide content increases, and substantially increases the local flavor of product.
Simultaneously, by enzymolysis solution is carried out two-stage ultrafiltration, realize the separation and purification of different product in enzymolysis solution, and carry out, for each point of subsegment product, the bone polysaccharide that following process obtains comprising chondroitin sulfate, the variant productions such as macromole polypeptide and micromolecule polypeptide, wherein gained content of chondroitin sulfate is higher than 92%, realize making full use of ossein enzymolysis solution, especially by by macromole polypeptide and wood sugar, halfcystine and VitB1 carry out Maillard reaction, intermediate product and the hot pressing product reaction of halfcystine and VitB1 that in reaction process, macromole polypeptide and wood sugar generation carbonyl ammonia react generate generate Mei Lade product, obtain flavor base material with rich flavor, result analysis according to GC-MS, levels of pyrazine in flavor base material is about 10 times of enzymolysis solution, aldoketones is about 2.5 times of enzymolysis solution, demonstrate the raw fragrant effect of Maillard reaction.The present invention realizes the recycling of waste while catering to the market requirement; and do not add any mineral acid, alkali; technical process is compact; processing parameter is accurate, and artificial interference factor is few, is applicable to enterprise scale and produces; make full use of low value chicken bone and obtain the multiple product with market outlook; realize the high value added utilization of chicken bone, reduce agricultural byproducts processing to improving business economic benefit while the pollution of environment, for the comprehensive utilization of chicken bone provides technical support.
Accompanying drawing explanation
Fig. 1 is the method process flow sheet of chicken bone coproduction collagen active peptide of the present invention and flavor base material;
Fig. 2 is hydrolysis degree change curve under the different enzymolysis time of stepwise discretization of the present invention reaction;
Fig. 3 is Sigma company chondroitin sulfate standard substance high-efficient liquid phase chromatogram;
Fig. 4 is the high-efficient liquid phase chromatogram of the chondroitin sulfate that the present invention extracts;
When Fig. 5 is different hot pressing extracting, different substances is with the variation diagram of hot pressing extracting time;
The one-tenth that Fig. 6 is bone meal of the present invention is grouped into table;
The one-tenth that Fig. 7 is animal oil of the present invention is grouped into table;
Fig. 8 is bone polysaccharide physical and chemical index analytical results cartogram of the present invention;
Fig. 9 is each point of subsegment ultrafiltration product and enzymolysis solution product oxidation-resistance cartogram;
Figure 10 is that maillard reaction product of the present invention becomes submeter.
Embodiment
Below in conjunction with accompanying drawing 1-10, the present invention is elaborated, can implement according to this after making those of ordinary skill in the art consult this specification sheets.
As shown in Figure 1, a kind of method of chicken bone coproduction collagen active peptide and flavor base material, it is characterized in that, chicken bone is carried out two sections of hot pressing extractings and obtains extract, drop into after extract is removed bone slag and leave standstill stratification in tank, shunting valve separation at the bottom of tank is utilized to obtain ossein and upper oil phase, and carry out stepwise discretization after carrying out high-pressure homogeneous process from the ossein of the extraction in extract, wherein said two sections of hot pressing method for extracting are: rinsed by chicken bone clear water, after removing surface bloodstain impurity, chicken bone and water being mixed according to 1: 1-2 mass ratio adds in hot pressure reaction tank, carry out one section of hot pressing extracting and two sections of hot pressing extractings in turn, wherein one section of hot pressing extraction temperature is 110-120 DEG C, extracting time 100-120min, two sections of hot pressing extraction temperatures are 130-140 DEG C, extracting time 70-90min,
In addition, also comprise the following steps:
Step one, stepwise discretization react, and are mixed with compound protease and flavor protease respectively according to sequencing by the ossein after high-pressure homogeneous process and carry out stepwise discretization reaction, obtain enzymolysis solution, stepwise discretization process carries out in a kettle., and carries out stirring at low speed, and rotating speed is 20-25r/min, to increase the touch opportunity of enzyme and substrate, it is to increase enzyme digestion reaction efficiency. in addition, described compound protease is a kind of enzyme mixed by multiple biological enzyme, comprise bromeline, papoid and neutral protease etc., described compound protease has multiple restriction enzyme site, there is multiple protein loci and cut off function, and can effective hydrophobic group in collagen protein enzymolysis, improve collagen protein solubleness, abundant enzymolysis is the former albumen of dissolved gum not easily, obtain a large amount of polypeptide and amino acid, and under the effect of flavor protease, peptide molecule chain end is modified, thus bitter peptides content in enzymolysis solution is controlled, fresh taste peptide content increases, improve the local flavor of product.
Step 2, two-stage ultrafiltration, the ultra-filtration membrane that gained enzymolysis solution employing molecular weight cut-off is 9-10kDa is carried out one-level ultrafiltration, obtain one-level and retain liquid and one-level filtrate, the ultra-filtration membrane that one-level filtrate employing molecular weight cut-off is 2-3kDa is carried out two-stage ultrafiltering, obtains second entrapment liquid and two grades of filtrates;Enzymolysis solution described in the present invention enters two-stage ultrafiltration coupling equipment after 200 order filter sieve filter, and ultrafiltration membrane elements molecular weight cut-off used is 10kDa, 2kDa respectively, and ultrafiltration temperature controls at 45 DEG C-50 DEG C, working pressure 0.5MPa. By enzymolysis solution is carried out two-stage ultrafiltration, realize the separation and purification in enzymolysis solution with different molecular weight product, obtaining > 10kDa, 10kDa-2kDa and < 2kDa tri-sections of materials, wherein > 10kDa main component is the precursor of bone polysaccharide and the part Maillard reaction comprising chondroitin sulfate; 10kDa-2kDa main component is macromole polypeptide, is the precursor of main Maillard reaction; < 2kDa is mainly micromolecule polypeptide, is rich in biological activity, carries out following process for the characteristic of each point of subsegment product and obtains variant production, it is achieved to making full use of of ossein enzymolysis solution. Each point of subsegment ultrafiltration product and enzymolysis solution product oxidation-resistance are shown in Fig. 9.
The preparation of step 3, flavor base material, gained one-level retains liquid adopts ethanol precipitation to process, leave standstill precipitation, get supernatant liquor and second entrapment liquid is mixed to form Maillard reaction precursor, hot pressure reaction is carried out after being mixed in hot pressure reaction still with a certain amount of wood sugar, halfcystine and VitB1 by gained Maillard reaction precursor, opening stirring at low speed in reaction process, rotating speed is 20-25r/min, obtains maillard reaction product; Gained maillard reaction product is carried out proceeds to vacuum concentration pot after interlayer water-bath is cooled to 60-70 DEG C and carries out vacuum concentration to Brix=40 ��, vacuum tightness is at more than 0.08MPa, and with spray-drier concentrated solution carried out after spraying dry both described flavor base material, wherein spray-drier feeding temperature is controlled to 180-190 DEG C, drop temperature is controlled to about 90 DEG C, and moisture content of finished products is not more than 5%.
The two grades of filtrates of gained in step 2 are carried out concentrate drying and had both obtained collagen active peptide by the preparation of step 4, collagen active peptide. Method therefor of the present invention is for carry out vacuum concentration to Brix=40 �� by two grades of filtrates, vacuum tightness is at more than 0.08MPa, and with spray-drier, concentrated solution is carried out spraying dry, wherein spray-drier feeding temperature is controlled to 180-190 DEG C, drop temperature is controlled to about 90 DEG C, moisture content of finished products is not more than 5%, the content of peptides obtaining collagen active peptide is about 91%, small molecules oligopeptide wherein is anti-oxidant and the function such as ACE suppression is remarkable, relative to the functional medicine of current synthetic, there is the features such as side effect is little, effect is remarkable.
In described chicken bone coproduction collagen active peptide and the method for flavor base material, described two sections of hot pressing extractive reactions carry out in hot pressure reaction tank, and after two sections of hot pressing extractive reactions terminate, carry out slight pressure release ftercompction, concrete grammar is: after two sections of hot pressing extractings terminate, open the pressure release valve 8-10min of hot pressure reaction tank, make in hot pressure reaction tank after decrease in temperature 5-10 DEG C, close pressure release valve 8-10min, make rise in temperature 5-10 DEG C to former temperature, and repeat 3-5 time according to this step. Process through slight pressure release ftercompction, the running balance in hot pressure reaction tank can be broken, promote the dynamic translation of material, improve the extract content of product, the present invention can the collagen protein such as the I-type collagen in high efficiency extraction os osseum and the II collagen type in cartilage, 100kg chicken bone can extract the ossein extract of about 360kgBrix4%, and wherein collagen content is about 40mg/g.
Total soluble substance in extract under different hot pressing extracting time conditions, crude protein and collagen content changed with the hot pressing extracting time, wherein total soluble substance is represented by TSS, chicken bone is the continuous stripping of material in it in hot pressing extractive process, wherein main material is protein and a small amount of solubility organic compound, as shown in Figure 5, total Soluble matter content has increase in various degree along with the raising of extracting time lengthening and extraction temperature, between different extraction temperature, total Soluble matter content changes from 0.9% to 5.2%, 1.9% to 5.6%, under differing temps, the change of total Soluble matter content is significantly, both P < 0.05, extraction temperature is 120 DEG C and when 130 DEG C between the different extracting time, total Soluble matter content is different, particularly 90min before extracting, total Soluble matter content has a big increase, increase not remarkable after 90min. crude protein content change significant difference between differing temps, P < 0.05, between different extraction temperature, crude protein content is changed to from 0.54% to 3.54%, 1.23% to 3.82%, when wherein extraction temperature is 120 DEG C, crude protein content amplification is maximum, extraction temperature is 120 DEG C and when 130 DEG C, before extracting, 90min crude protein incremental amplitude is big, after 90min, amplification tends towards stability, when extraction temperature is 120 DEG C, front 20min changes slowly, after extracting 20min, its content sharply increases until the trend that significantly increases in addition during 120min, illustrate that chicken bone also exists many undissolved collagen proteins.
In described chicken bone coproduction collagen active peptide and the method for flavor base material, in step one, the quality of added compound protease and flavor protease is respectively the 0.2-0.3% of ossein quality used, enzyme digestion reaction temperature is 51-53 DEG C, each step enzyme digestion reaction carries out 100-120min respectively, and each step enzyme digestion reaction is warming up to 90-100 DEG C respectively and keeps 20-30min to carry out enzyme-deactivating after terminating; In addition, in stepwise discretization process, enzymolysis solution is carried out stirring at low speed.
The condition of described enzyme digestion reaction obtains through test of many times checking, and extract is divided into many parts be hydrolyzed 1h, 2h, 3h, 4h, 5h respectively with different biological enzyme, and degree of hydrolysis (DH) is affected as shown in Figure 2 by hydrolysis time. Degree of hydrolysis constantly increases along with the prolongation of hydrolysis time, and after hydrolysis exceedes certain time, hydrolysis rate becomes slow, and degree of hydrolysis ascensional range reduces, and is due to the prolongation with hydrolysis time, and concentration of substrate reduces or caused by enzyme activity decline. Papoid, conjugated protein and neutral protease are before hydrolysis during 3h, and before degree of hydrolysis rapid development illustrates, 3h hydrolysis reaction is violent, and protein is degraded into free amino acid in a large number. And the rising tendency of degree of hydrolysis becomes mild after 3h. Flavor protease before hydrolysis during 2h degree of hydrolysis increase slowly, after 2h, hydrolysis reaction is violent, and after hydrolysis 4h, degree of hydrolysis increases and is tending towards saturated. Although hydrolysis time extends is conducive to the thorough hydrolysis of albumen, but after hydrolysis exceedes certain time, degree of hydrolysis rising tendency is tending towards saturated, and the more long power consumption of hydrolysis time is more big. Therefore, comprehensive degree of hydrolysis and energy consumption determine that flavor protease and the best enzymolysis time of compound protease are respectively about 2h.
In described chicken bone coproduction collagen active peptide and the method for flavor base material, the concrete grammar of ethanol precipitation described in step 3 is: described one-level retained after liquid mixes according to the volume ratio of 1: 2-3 with 90-100% ethanol, centrifugal through 8000-10000r/min, obtain supernatant and lower sediment.After ethanol precipitation gained lower sediment is processed 2-3 time with 90-100% ethanol dehydration, obtain the bone polysaccharide containing more than 92% chondroitin sulfate after drying. Described bone polysaccharide physical and chemical index analytical results is shown in Fig. 8; Fig. 3 is the high-efficient liquid phase chromatogram of chondroitin sulfate standard substance; Fig. 4 is the high-efficient liquid phase chromatogram of the chondroitin sulfate that the present invention extracts, and is 92.1% through calculating content of chondroitin sulfate in gained bone polyoses extract of the present invention.
In described chicken bone coproduction collagen active peptide and the method for flavor base material, in step 3, the quality of added wood sugar, halfcystine and VitB1 is respectively the 0.4-0.6% of Maillard reaction precursor mass used, described hot pressure reaction temperature is 100-110 DEG C, and the hot pressure reaction time is 80-100min. the Maillard reaction precursor formed with second entrapment liquid and ethanol precipitation gained supernatant liquid is at wood sugar, Maillard reaction is carried out under the participation of halfcystine and VitB1, wherein wood sugar provides carbonyl, halfcystine and VitB1 are main meat-like flavor precursors, intermediate product and the pyrolysis product reaction of halfcystine and VitB1 that in reaction process, the polypeptide in gained Maillard reaction precursor and wood sugar generation carbonyl ammonia react generate generate maillard reaction product with rich flavor, and obtain flavor base material through concentrate drying, result analysis according to GC-MS, acid class and letones are less with the change of enzymolysis time relative content, levels of pyrazine in gained flavor base material is about 10 times of enzymolysis solution, Pyrazine material mostly has barbecue taste, make enzymolysis product thick in meat flavor, aldoketones is about 2.5 times of enzymolysis solution, further enhancing the meat taste of enzymolysis solution and fruital taste, and under the effect of the additives such as wood sugar, halfcystine and VitB1, Maillard reaction strengthens the local flavor of enzymolysis solution so that product special flavour and function are all good. the composition of described maillard reaction product forms as shown in Figure 10, demonstrates the raw fragrant effect of Maillard reaction.
In described chicken bone coproduction collagen active peptide and the method for flavor base material, the extracting method of described ossein is: carry out stratification after gained extract screens out bone slag, remove after upper oil phase both described ossein; In addition, ossein is carried out high-pressure homogeneous method is: adopt high pressure homogenizer to carry out high-pressure homogeneous to ossein, wherein sets homogenizing temperature 70 �� 2 DEG C, pressure 30 �� 2MPa, rotating speed 700-800r/min, homogenizing time 5-8min. The comprehensive actions such as liquid stream strong, reciprocal in homogenizing process is sheared, friction, centrifugal extruding and liquid stream collision, promote that in ossein, collagen protein spirals is understood poly-, increase its solvability and peptide chain gap, for follow-up stepwise discretization provides condition, found that through high-pressure homogeneous ossein degree of hydrolysis after enzymolysis terminates be 23.4%, higher by more than 6% than without high-pressure homogeneous ossein enzymolysis solution degree of hydrolysis.
In described chicken bone coproduction collagen active peptide and the method for flavor base material, adopting vibratory screening apparatus division to carry out bone slag and screen out, be rich in hydroxyapatite in described bone slag, vibratory screening apparatus aperture used is 40-50 order. After hot pressing extracting terminates, major part bone slag is deposited in the bottom of hot pressing extracting tank, small portion bone slag pumps with the pressure pump of ossein through hot pressing extracting tank, this part the bone slag being so blended in ossein needs to screen out through vibratory screening apparatus, and can will screen out bone slag remaining in the bone slag and hot pressure reaction tank that obtain together, being prepared as bone meal through pulverizing drying, for animal-feed or farmland inorganic fertilizer, wherein calcium, phosphorus content are respectively 62.3% and 29.4%.The composition of described bone meal forms as shown in Figure 6.
In described chicken bone coproduction collagen active peptide and the method for flavor base material, get the upper oil phase after stratification and upper oil phase is heated to about 80 DEG C, add the 90-95 DEG C of hot water that volume is upper oil phase 10-15%, 10-15r/min stirs 8-10min, remove aqueous phase after standing sedimentation 20-30min, surplus oil heat phase is obtained animal oil to being cooled to rapidly 80-85 DEG C within 30min after 100-115 DEG C. The composition of described animal oil forms as shown in Figure 7. As shown in Figure 7, the animal oil product being made up of chicken bone reaches edible blend oil standard substantially, and meat-like flavor is strong, and nutritive value height, can be used for oleomargarine and flavor oil etc.
Embodiment 1
Step one, 300kg chicken bone clear water is rinsed, remove surface bloodstain impurity, it is divided into three batches to drop in hot pressure reaction tank respectively and add quantitative clear water according to the mass ratio of 1: 2, carry out two sections of hot pressing extractings, one section of hot pressing extraction temperature is 120 DEG C, extracting time 120min, two sections of hot pressing extraction temperatures are 130 DEG C, extracting time 90min, period slight pressure release/ftercompction improves product and puies forward rate, method is: after two sections of hot pressing extractings terminate, open the pressure release valve 10min of hot pressure reaction tank, make to close pressure release valve 10min after decrease in temperature 5 DEG C in hot pressure reaction tank, and make rise in temperature 5 DEG C return back to former temperature, 3 times are repeated according to this step.
Step 2, extract is adopted vibratory screening apparatus division remove bone slag, vibratory screening apparatus aperture is 40 orders, entering standing tank to leave standstill, utilize diverting valve separation ossein and upper oil phase, ossein enters enzyme digestion reaction still through high pressure homogenizer when 30 �� 2MPa after homogeneous depolymerization.
Step 3, ossein adopt stepwise discretization method carry out enzymolysis, compound protease and flavor protease is successively added by the 0.2% of substrate quality, two step enzyme digestion reaction temperature are 51-53 DEG C, two step enzyme digestion reactions carry out 120min respectively, two step enzyme digestion reactions are warming up to 90 DEG C respectively after terminating and keep 20min to carry out enzyme-deactivating, enzymolysis process is opened stirring at low speed, rotating speed 20��25r/min in reactor.
Step 3, enzymolysis solution enter two-stage ultrafiltration coupling equipment after 200 order filter sieve filter, and ultrafiltration membrane elements molecular weight cut-off is 10kDa, 2kDa respectively, and ultrafiltration temperature controls at 45 DEG C-50 DEG C, working pressure 0.5MPa.
Step 4, described one-level retained liquid mix according to the volume ratio of 1: 3 with 95% ethanol after, centrifugal through 10000r/min, obtain supernatant and lower sediment, lower sediment continues to dewater after 2 times with 95% ethanolic soln, drying obtains the bone polysaccharide finished product containing chondroitin sulfate, and supernatant liquid adds second entrapment liquid and forms Maillard reaction precursor.
Step 5, by Maillard reaction precursor move into hot pressure reaction still, add the wood sugar of Maillard reaction precursor quality 0.5%, halfcystine and VitB1 respectively, hot pressure reaction 90min at 105 DEG C, open stirring at low speed, the Mei Lade product obtained, interlayer water-bath proceeds to vacuum concentration pot and carries out vacuum concentration to Brix=40 �� after being cooled to 60-70 DEG C, vacuum tightness is at more than 0.08MPa, with spray-drier, concentrated solution is dry, obtain flavor base material.
Step 6, two grades of filtrate vacuum concentration dryings are obtained collagen active peptide; In the bone slag screened out in extract and hot pressure reaction tank, remaining bone slag makes bone meal after micronizing drying, can be used for animal-feed and farmland inorganic fertilizer;Animal oil transfers to animal oil hold-up vessel by shunting valve, 90 DEG C of hot water of 15% are added in the animal oil of about 80 DEG C temperature, 10-15r/min stirs 10min, standing sedimentation 30min abandons waste water, animal oil is heated to 115 DEG C and removes moisture, being cooled to rapidly 80-85 DEG C with interlayer water-bath, temperature fall time controls in 30min, obtains finished chicken animal oil.
Although embodiment of the present invention are open as above, but listed utilization that it is not restricted in specification sheets and enforcement mode, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore claim is not being deviated from and under general concept that equivalency range limits, the present invention is not limited to specific details and illustrates and the legend described here.
Claims (8)
1. the method for a chicken bone coproduction collagen active peptide and flavor base material, it is characterised in that,
Chicken bone is carried out two sections of hot pressing extractings and obtains extract, and carry out stepwise discretization after the ossein extracted from extract is carried out high-pressure homogeneous process, wherein said two sections of hot pressing method for extracting are: mixed according to 1:1-2 mass ratio with water by chicken bone, carry out one section of hot pressing extracting and two sections of hot pressing extractings in turn, wherein one section of hot pressing extraction temperature is 110-120 DEG C, extracting time 100-120min, two sections of hot pressing extraction temperatures are 130-140 DEG C, extracting time 70-90min;
Wherein, described two sections of hot pressing extractive reactions carry out in hot pressure reaction tank, and after two sections of hot pressing extractive reactions terminate, carry out slight pressure release ftercompction, concrete grammar is: after two sections of hot pressing extractings terminate, open the pressure release valve 8-10min of hot pressure reaction tank, make to close after decrease in temperature 5-10 DEG C in hot pressure reaction tank pressure release valve 8-10min, and make rise in temperature 5-10 DEG C, repeat 3-5 time according to this step;
In addition, also comprise the following steps:
Step one, stepwise discretization react, and are mixed with compound protease and flavor protease respectively according to sequencing by the ossein after high-pressure homogeneous process and carry out stepwise discretization reaction, obtain enzymolysis solution;
Step 2, two-stage ultrafiltering, the ultra-filtration membrane that gained enzymolysis solution employing molecular weight cut-off is 9-10kDa is carried out one-level ultrafiltration, obtain one-level and retain liquid and one-level filtrate, the ultra-filtration membrane that one-level filtrate employing molecular weight cut-off is 2-3kDa is carried out two-stage ultrafiltering, obtains second entrapment liquid and two grades of filtrates;
The preparation of step 3, flavor base material, gained one-level retains liquid adopts ethanol precipitation to process, leave standstill precipitation, get supernatant liquor and second entrapment liquid is mixed to form Maillard reaction precursor, hot pressure reaction is carried out after being mixed with a certain amount of wood sugar, halfcystine and VitB1 by gained Maillard reaction precursor, obtain maillard reaction product, by after gained maillard reaction product concentrate drying both described flavor base material;
The two grades of filtrates of gained in step 2 are carried out concentrate drying and had both obtained collagen active peptide by the preparation of step 4, collagen active peptide.
2. the method for chicken bone coproduction collagen active peptide as claimed in claim 1 and flavor base material, it is characterized in that, in step one, the quality of added compound protease and flavor protease is respectively the 0.2-0.3% of ossein quality used, enzyme digestion reaction temperature is 51-53 DEG C, each step enzyme digestion reaction carries out 100-120min respectively, and each step enzyme digestion reaction is warming up to 90-100 DEG C respectively and keeps 20-30min to carry out enzyme-deactivating after terminating.
3. the method for chicken bone coproduction collagen active peptide as claimed in claim 1 and flavor base material, it is characterized in that, the concrete grammar of ethanol precipitation described in step 3 is: described one-level retained after liquid mixes according to the volume ratio of 1:2-3 with 90-100% ethanol, centrifugal through 8000-10000r/min, obtain supernatant and lower sediment.
4. the method for chicken bone coproduction collagen active peptide as claimed in claim 3 and flavor base material, it is characterised in that, after ethanol precipitation gained lower sediment is processed 2-3 time with 90-100% ethanol dehydration, obtain chondroitin sulfate after drying.
5. the method for chicken bone coproduction collagen active peptide as claimed in claim 1 and flavor base material, it is characterized in that, in step 3, the quality of added wood sugar, halfcystine and VitB1 is respectively the 0.4-0.6% of Maillard reaction precursor mass used, described hot pressure reaction temperature is 100-110 DEG C, and the hot pressure reaction time is 80-100min.
6. the method for chicken bone coproduction collagen active peptide as claimed in claim 1 and flavor base material, it is characterised in that, the extracting method of described ossein is: carry out stratification after gained extract screens out bone slag, remove after upper oil phase both described ossein;
In addition, ossein is carried out high-pressure homogeneous method is: adopt high pressure homogenizer to carry out high-pressure homogeneous to ossein, wherein sets homogenizing temperature 70 �� 2 DEG C, pressure 30 �� 2MPa, rotating speed 700-800r/min, homogenizing time 5-8min.
7. the method for chicken bone coproduction collagen active peptide as claimed in claim 6 and flavor base material, it is characterized in that, adopt vibratory screening apparatus division that extract is carried out bone slag to screen out, vibratory screening apparatus aperture used is 40-50 order, and can through pulverizing, drying is prepared as bone meal by remaining bone slag in the bone slag that screens out and hot pressure reaction tank.
8. the method for chicken bone coproduction collagen active peptide as claimed in claim 7 and flavor base material, it is characterized in that, get the upper oil phase after stratification and upper oil phase is heated to about 80 DEG C, add the 90-95 DEG C of hot water that volume is upper oil phase 10-15%, 10-15r/min stirs 8-10min, remove aqueous phase after standing sedimentation 20-30min, surplus oil heat phase is obtained animal oil to being cooled to 80-85 DEG C within 30min after 100-115 DEG C.
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| CN111567671A (en) * | 2020-06-17 | 2020-08-25 | 江苏特味浓生物技术开发有限公司 | Chicken bone protein gel, chicken bone protein gel stuffing and preparation method |
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| CN112725407A (en) * | 2021-01-20 | 2021-04-30 | 河南恒都生物科技开发有限公司 | Digestion characteristic evaluation method of bovine bone collagen polypeptide |
| CN117265020B (en) * | 2023-11-21 | 2024-02-20 | 烟台融科生物科技有限公司 | Method for co-producing pig bone essence and bone collagen active peptide by using pig bone |
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