CN102754739A - Preparation method of composite peptide-copper chelate by utilizing meat processing byproduct - Google Patents
Preparation method of composite peptide-copper chelate by utilizing meat processing byproduct Download PDFInfo
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Abstract
The invention provides a preparation production method of a composite peptide-copper chelate by utilizing a meat processing byproduct and a corresponding product composite peptide-copper chelate. The preparation method of the composite peptide-copper chelate comprises the following steps: carrying out enzymolysis on the meat processing byproduct (blood powder, feather meal and the like) with proteolytic enzyme in a certain condition to obtain enzymatic hydrolysate with small peptide as a main component; carrying out a chelation reaction on a copper salt solution and the enzymatic hydrolysate serving as ligand, and controlling the temperature, pH and reaction time of a reaction system so as to prepare a better chelated product through a two-step chelation reaction by adopting a method of determining a charge rate according to the copper ion coordination characteristics and small peptide detection result for the first time. The product composite peptide-copper chelate can be effectively absorbed by animals including ruminant, livestock and aquatic animals, so that the application range of byproducts can be enlarged, and the utilization rate of the byproducts can be improved. The preparation method is less in investment, and is easy to produce on large scale.
Description
Technical field
The present invention relates to a kind of production method of novel animal feed additive, specifically, relate to a kind of compound peptide copper chelate and production method thereof, belong to the animal feed additive field.
Background technology
Copper is the constituent and the activator of many enzymes in the animal body as one of essential trace element of animal, participates in hair growth and pigmentation, keeps the animal reproduction function, regulates body neuro-humoral mechanism and immune response; Simultaneously copper also is one of composition that constitutes hemoglobin, influences the hematopoiesis function of body iron through blue copper protein, and erythrocytic generation must have the existence of copper.Therefore, if lack copper, then pathological phenomenons such as anaemia, ataxia, abnormal bone metabolism can occur, thereby influence nutrient metabolism and the growth and development state of animal.According to the animal physiological function scientific and reasonable in feed, add copper; Both can satisfy the basic nutritional need of animal, and avoid copper to lack and cause various illnesss, and can effectively improve the production reproductive performance of animal again copper; Improve immunity, promote its healthy growth and development.
The development of copper additive product can be divided into for four generations: first generation product is an inorganic salts copper additive, like copper sulphate etc.Second generation copper additive is simple organic acid salt, like copper salts such as gluconic acid, citric acids.There is a lot of drawbacks in this two series products in application: the one, and influence such as the antagonism of pH value, inorganic ions, organic macromolecule etc. can't be by complete absorption in the poor stability, factor receptor; The 2nd, big to the animal intestines and stomach excitant, the activity of vitamin, little ecology etc. influences digestibility in the destructible feed; The 3rd, animal absorbs less, and major part excretes, and contaminated soil and water source are bigger to environmental disruption property; The 4th, a large amount of copper are deposited in the liver of animal, very easily deposit after the human consumption, even cause poisoning, become the dangerous matter sources of food security.Third generation copper additive is the single amino acid chelate; Though have biological stability strong, advantage such as be prone to digested and assimilated, effect is not remarkable in practical application, this is because animal organism needs diversified organic chelate; Single specific chelate demand is less; Add the competition that too much not only is prone to cause absorbing path, influence absorbing of other amino acid and copper, and cause waste.In addition, single amino acid chelate production cost is higher, has increased aquaculture cost.The little peptide copper of the 4th generation copper additive chelate becomes the focus of concern.
Modern science is thought; The little Toplink of being made up of 2 or 3 amino acid residues intactly gets into the body circulation through intestinal mucosa cells; Absorption has that transport speed is fast, power consumption is low, carrier is difficult for saturated; With advantages such as the absorption of free amino acid are uncontested, and uncontested property of transhipment and inhibition between the various peptide.Animal tissue can directly utilize the amino acid synthetic tissue albumen in the little peptide.Little peptide copper chelate is that the absorption ALT-CH alternate channel by little peptide is absorbed and used, and can promote the absorption of copper, more helps the raising of copper biological value.
China's animal husbandry in recent years and the development of carnivorous processing industry are rapid, and the high-valued comprehensive utilization of a large amount of animal bloods, feather the like waste becomes the focus of research.The at present topmost approach that utilizes is to become forage protein blood cell powder, feather meal etc. through simple processing and preparing, but animal is low to these animal protein feed digestibilities, and feeding value is not high; And China's regulation animal protein feed is forbidden to be applied to ruminant, has limited the range of application of product.The existing at present report that carnivorous processing byproduct is used to prepare compound peptide microelement chelate; But enzyme solution treatment process behind alkaline hydrolysis method that adopts or the first alkaline hydrolysis; Not only can destroy the amino acid active in the product, reduce the nutritive value of product, and having relatively high expectations to production equipment; The waste liquid environmental pollution that produces is bigger, and therefore the gentle copper composite peptide chelate complex production technology efficiently of exploitation becomes the task of top priority of the carnivorous processing byproduct of comprehensive utilization.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of compound peptide copper chelate newly; This method is a raw material with carnivorous processing byproduct; Produce compound peptide copper chelate through biological enzymolysis technology, carnivorous processing byproducts such as comprehensive development and utilization blood, feather improve feeding added value.
The present invention provides a kind of production method of compound peptide copper chelate, and medium and small peptide of this method and copper rate of charge are to calculate according to copper ion coordination characteristic and little peptide testing result, and more science is accurate, and the products obtained therefrom chelating is better.
The present invention provides a kind of production method of compound peptide copper chelate, and this preparation method is prone to row, and is simple to operate, little to the production equipment corrosiveness, is easy to large-scale production.
The present invention provides a kind of compound peptide copper chelate, its stable in animal body easy absorption, and it is low to consume energy, and can satisfy the needs of animal body to diversified organic chelate, effectively promotes breeding performonce fo animals.
It is the production method of the compound peptide copper chelate of raw material with carnivorous processing byproduct that the present invention provides a kind of; This method utilizes animal proteolytic enzyme carnivorous processing byproducts such as enzymolysis blood, feather under optimum condition to prepare enzymolysis liquid; The enzymolysis liquid main component is little peptide, oligopeptides and few partial amino-acid that can directly be absorbed by animal, enzymolysis liquid is mixed through chelatropic reaction making the compound peptide copper chelate product that can effectively be absorbed by animal then with copper ion solution.
The present invention provides a kind of production method of compound peptide copper chelate, comprises the steps:
(1) in raw material, add an amount of water, it is 10～30% the aqueous solution that raw material is made into mass concentration, and fully mixing is transferred system pH to stirring non-resistance with sodium hydroxide solution, adds an amount of animal proteolytic enzyme after having transferred, mixing, and the constant temperature enzymolysis gets enzymolysis liquid.Wherein the enzymatic hydrolysis system optimal pH 7～10, and the protease addition is 500～1000U/g substrate quality, and hydrolysis temperature is 40～50 ℃, and enzymolysis time is 20h～30h;
(2) the inorganic mantoquita that will select for use is dissolved in an amount of water and forms the aqueous solution; Constantly stir and suitable temperature conditions under; According to calculating the gained rate of charge; In the above-mentioned copper ion aqueous solution, add the compound peptide solution of a great deal of, continued stirring reaction 1～2 hour, keeping system pH in the course of reaction is 3.5～4.5;
(3) reaction finishes the back and product is carried out centrifugal, separates;
(4) it is neutral separating afterreaction liquid accent ph, transfers to 60～80 ℃ of preference temperatures, and the continuation reaction is 1～2 hour under stirring condition, and it is the best that course of reaction keeps reaction system pH6.5～7, and reaction end back is carried out centrifugal to product, separate;
(5) the two-step reaction product drying is handled, and makes compound peptide-copper chelate finished product.
The present invention can select the copper inorganic salts used always, such as copper sulphate, and copper chloride etc.
Among the present invention, according to mantoquita coordination characteristic, the compound peptide solution that in reaction system, adds equivalent according to the ratio of coordinating group and metal ion mol ratio 4:1 is good.
The dried of the compound peptide copper of gained of the present invention chelate product can adopt modes such as air-dry, freezing and vacuum drying to carry out, and adopts low temperature drying best, and is because can keep the good outward appearance of product like this, mobile and stable.
It is raw material that the present invention adopts carnivorous processing byproduct; Utilize protease with the raw material enzymolysis, compare, more can protect the amino acid active in the product with enzyme solution treatment process behind alkaline hydrolysis method that adopted or the first alkaline hydrolysis in the past; Guarantee the nutritive value of product, reduce the loss of production equipment.
It is raw material that the present invention adopts carnivorous processing byproduct, utilizes protease with the raw material enzymolysis, and gained enzymolysis liquid main component is little peptide, oligopeptides and few partial amino-acid that can directly be absorbed by animal; Enzymolysis liquid and the compound peptide copper of copper ion chelatropic reaction products obtained therefrom chelate product are stable in animal body to be prone to absorb; It is low to consume energy, and can satisfy the needs of animal body to diversified organic chelate, can effectively be absorbed by animal; Promote breeding performonce fo animals, improved utilization rate greatly.And this series products can be used to comprise ruminant, and fowl poultry, aquatic livestock etc. have enlarged the purposes of carnivorous processing byproduct or animal protein in interior animal feed.
The production method of compound peptide copper chelate provided by the invention is configured to solution with copper salt earlier, with the part reaction, helps chelatropic reaction and carries out full and uniform fast again; Peptide and copper rate of charge be not picture in the past product add according to weight ratio, but calculate by concrete coordination characteristic of copper ion and the medium and small peptide testing result of enzymolysis liquid analysis-by-synthesis, more science is accurate, products obtained therefrom chelating degree is better.This preparation method is prone to row, and is simple to operate, little to the production equipment corrosiveness, is easy to large-scale production.In addition, the present invention adopts two step chelatings, and chelatropic reaction is abundant, and the preparation of product yield is high.
The specific embodiment
Embodiment 1:
With carnivorous processing byproduct blood cell powder, anhydrous cupric sulfate is the compound peptide-copper chelate of feedstock production, and concrete preparation process is following:
(1) in raw material blood cell powder, adds an amount of water; It is 20% the aqueous solution that raw material is made into mass concentration; Fully mixing is to stirring non-resistance, and using 20% sodium hydroxide solution to transfer system pH is 8.5, adds the protease of 800U/g substrate quality after having transferred; Mixing, 40 ℃ of insulation enzymolysis got enzymolysis liquid in 20 hours;
(2) take by weighing a certain amount of cupric sulfate pentahydrate; Add distilled water (distilled water: the cupric sulfate pentahydrate weight ratio is 1:1), stirring and dissolving, temperature of reaction system is 40 ℃; Continue under the stirring condition; According to each little peptide content in the enzymolysis blood cell powder, the enzymolysis blood cell powder solution that in reaction system, adds equivalent according to the ratio of coordinating group and metal ion mol ratio 4:1 continued stirring reaction 1 hour, and using sodium hydroxide solution to keep system pH in the course of reaction is about 4;
(3) product is centrifugalized purifying;
(4) it is neutral separating afterreaction liquid accent ph, and system temperature transfers to 80 ℃, under stirring condition, continues reaction 1.5 hours, and it is neutrality that course of reaction keeps reaction system pH;
(5) reaction finish the back product is carried out centrifugal, separation and purification, the reactant liquor reusable edible after final the processing;
(6) the two-step reaction product merges, and adopts low temperature drying to handle and obtains solid product.
Technology gained enzymolysis blood cell powder chelated copper product yield of the present invention is about 92%, and product copper content is 10.7%.Be about 62% through kjeldahl determination quantitative analysis product crude protein content.Water-solubility protein accounts for more than 98% in the enzymolysis blood cell powder solution, wherein is prone to absorbed little peptide and oligopeptides content more than 90%; The molecule quantitative change is big behind little peptide and the copper chelating, and dissolubility diminishes, and from solution, separates out, and separates thereby be convenient to product.Enzymolysis blood cell powder chelated copper product is carried out enzymolysis experiment, survey its water-soluble protein content and be merely about 1%, separate out after further specifying peptide and copper chelating, rather than simply saltout, and product chelating effect is fine.
Embodiment 2:
With carnivorous processing byproduct blood meal, anhydrous cupric sulfate is the compound peptide-copper chelate of feedstock production, and concrete preparation process is following:
(1) in the raw material blood meal, add an amount of water, it is 20% the aqueous solution that raw material is made into mass concentration, and fully mixing is to stirring non-resistance; Using 20% sodium hydroxide solution to transfer system pH is 8.5; The protease that adds 800U/g substrate quality after having transferred, mixing, 40 ℃ of insulation enzymolysis got enzymolysis liquid in 20 hours;
(2) take by weighing a certain amount of cupric sulfate pentahydrate; Add distilled water (distilled water: the cupric sulfate pentahydrate weight ratio is 3:1), stirring and dissolving, temperature of reaction system is 50 ℃; Continue under the stirring condition; According to the medium and small peptide equal size of blood meal enzymolysis liquid, the enzymolysis blood meal solution that in reaction system, adds equivalent according to the ratio of coordinating group and metal ion mol ratio 4:1 continued stirring reaction 2 hours, and using sodium hydroxide solution to keep system pH in the course of reaction is about 5;
(3) reaction centrifugalizes purifying to product after finishing;
(4) separating afterreaction liquid accent ph is about 7, and system temperature transfers to 80 ℃, under stirring condition, continues reaction 2 hours, and it is neutral that course of reaction keeps reaction system pH;
(5) reaction finish the back product is carried out centrifugal, separation and purification;
(6) the two-step reaction product merges, and adopts low temperature drying to handle and obtains solid product.Rest solution can recycle in the next round reaction after reaction system was isolated product.
Technology gained enzymolysis blood meal chelated copper product yield of the present invention is about 89%, and product copper content is 9.5%.Be about 67% through kjeldahl determination quantitative analysis product crude protein content.Water-solubility protein accounts for more than 80% in the enzymolysis blood meal solution, wherein is prone to absorbed little peptide and oligopeptides content more than 90%.The molecule quantitative change is big behind little peptide and the copper chelating, and dissolubility diminishes, and from solution, separates out, and separates thereby be convenient to product.Enzymolysis blood meal chelated copper product is carried out enzymolysis experiment, survey its water-soluble protein content, separate out after further specifying peptide and copper chelating, rather than simply saltout, and product chelating effect is fine less than 3%.
Embodiment 3:
With carnivorous processing byproduct feather meal, copper chloride is the compound peptide-copper chelate of feedstock production, and concrete preparation process is following:
(1) in the raw material feather meal, adds an amount of water; It is 20% the aqueous solution that raw material is made into mass concentration; Fully mixing is to stirring non-resistance, and using 20% sodium hydroxide solution to transfer system pH is 8.5, adds the protease of 1000U/g substrate quality after having transferred; Mixing, 40 ℃ of insulation enzymolysis got enzymolysis liquid in 30 hours;
(2) take by weighing a certain amount of copper chloride; Add distilled water (distilled water: the copper chloride weight ratio is 3:1), stirring and dissolving, temperature of reaction system is 50 ℃; Continue under the stirring condition; According to the medium and small peptide equal size of blood meal enzymolysis liquid, the enzymolysis blood meal solution that in reaction system, adds equivalent according to the ratio of coordinating group and metal ion mol ratio 4:1 continued stirring reaction 2 hours, and using sodium hydroxide solution to keep system pH in the course of reaction is about 5;
(3) reaction centrifugalizes purifying to product after finishing;
(4) separating afterreaction liquid accent ph is about 7, and system temperature transfers to 80 ℃, under stirring condition, continues reaction 2 hours, and it is neutral that course of reaction keeps reaction system pH;
(5) reaction finish the back product is carried out centrifugal, separation and purification;
(6) the two-step reaction product merges, and adopts low temperature drying to handle and obtains solid product.Rest solution can recycle in the next round reaction after reaction system was isolated product.
Technology gained enzymolysis blood meal chelated copper product yield of the present invention is about 85%, product copper content 9.2%.Be about 67% through kjeldahl determination quantitative analysis product crude protein content.Water-solubility protein accounts for more than 80% in the enzymolysis blood meal solution, wherein is prone to absorbed little peptide and oligopeptides content more than 90%.The molecule quantitative change is big behind little peptide and the copper chelating, and dissolubility diminishes, and from solution, separates out, and separates thereby be convenient to product.Enzymolysis blood meal chelated copper product is carried out enzymolysis experiment, survey its water-soluble protein content, separate out after further specifying peptide and copper chelating, rather than simply saltout, and product chelating effect is fine less than 3%.
Existing technology generally adopts the volume drying or the back alcohol of saltouing to wash when product separates purification; The former can not separate product with raw material; Latter's alcohol wash can with the part not the copper of chelating separate with chelate; Still possibly have a large amount of not peptide raw materials of chelating in the product, real composite peptide chelate complex content is lower in the product.The material liquid soluble protein is more than 98% in the technology of the present invention; Behind little peptide and the copper chelating, because molecular change is big, dissolubility diminishes and separates out; Product separates the not chelating of a small amount of absorption is removed in the back with a small amount of pure flush away copper ion with reaction system; To purifying products, and through the non-reaction of saltouing of further enzymolysis experimental verification, thereby obtain than the better product of existing technology chelating.
Claims (4)
1. method of utilizing carnivorous processing byproduct to prepare compound peptide-copper chelate, it is characterized in that: with carnivorous processing byproduct blood cell powder, blood meal, feather meal etc. is raw material, makes enzymolysis liquid through enzymolysis, as part; Copper is configured to the solution with part generation chelatropic reaction; Through compound peptide-copper chelates of preparation such as two step chelatropic reactions, centrifugal, analysis, dryings.
2. the carnivorous processing byproduct of utilization according to claim 1 prepares the method for compound peptide-copper chelate, comprises following content:
(1) in raw material, add an amount of water, it is 10～30% the aqueous solution that raw material is made into mass concentration, and fully mixing is transferred system pH to stirring non-resistance with sodium hydroxide solution, adds an amount of animal proteolytic enzyme after having transferred, mixing, and the constant temperature enzymolysis gets enzymolysis liquid; Wherein the enzymatic hydrolysis system optimal pH 7～10, and the protease addition is 500～1000U/g substrate quality, and hydrolysis temperature is 40～50 ℃, and enzymolysis time is 20h～30h;
(2) the inorganic mantoquita that will select for use is dissolved in an amount of water and forms the aqueous solution; Constantly stir and suitable temperature conditions under; According to calculating the gained rate of charge; In the above-mentioned copper ion aqueous solution, add the compound peptide solution of a great deal of, continued stirring reaction 1～2 hour, keeping system pH in the course of reaction is 3.5～4.5;
(3) reaction finishes the back and product is carried out centrifugal, separates;
(4) it is neutral separating afterreaction liquid accent ph, transfers to 60～80 ℃ of preference temperatures, and the continuation reaction is 1～2 hour under stirring condition, and it is the best that course of reaction keeps reaction system pH6.5～7, and reaction end back is carried out centrifugal to product, separate;
(5) the two-step reaction product drying is handled, and makes compound peptide-copper chelate finished product, and wherein the present invention can select the copper inorganic salts used always, such as copper sulphate, and copper chloride etc.
3. according to the production method of right 2 said a kind of compound peptide copper chelates, medium and small peptide of this method technology and copper rate of charge are to calculate according to copper ion coordination characteristic and little peptide testing result, and more science is accurate, and the products obtained therefrom chelating is better.
4. according to the production method of right 2 said a kind of compound peptide copper chelates, it is characterized in that: through two step chelatropic reactions, chelatropic reaction is abundant, and solution recycle behind the chelatropic reaction, and chelatropic reaction is abundant, and raw material availability and product yield are high.
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| CN104585513A (en) * | 2015-02-06 | 2015-05-06 | 江苏三仪生物工程有限公司 | Production method for feather oligopeptide chelating type mineral element |
| CN105661049A (en) * | 2016-03-17 | 2016-06-15 | 上海源耀生物股份有限公司 | Polypeptide copper chelate prepared by using soybean protein isolate as substrate and preparation method |
| CN105967761A (en) * | 2016-05-26 | 2016-09-28 | 陈可夫 | Method for producing amino acid water-soluble fertilizer by utilizing Drawida Japonica Michelsen |
| CN106538844A (en) * | 2016-11-26 | 2017-03-29 | 青岛中泰和生物科技有限公司 | A kind of preparation method of marine protein peptide chelated copper |
| CN108218952A (en) * | 2017-12-31 | 2018-06-29 | 连云港大海饲料有限公司 | A kind of preparation method of green feed additive chelating copper ions peptide |
| CN112299930A (en) * | 2020-01-07 | 2021-02-02 | 青岛帝保隆微碳农业技术有限公司 | High-concentration suspended calcium-magnesium fertilizer and preparation method thereof |
| CN112592239A (en) * | 2020-02-06 | 2021-04-02 | 山东世纪瑞文信息技术有限公司 | Seaweed calcium magnesium fertilizer and preparation method thereof |
| CN115215920A (en) * | 2022-07-29 | 2022-10-21 | 重庆工商大学 | Method for preparing small peptide chelated copper by using waste printed circuit board |
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| CN104585513A (en) * | 2015-02-06 | 2015-05-06 | 江苏三仪生物工程有限公司 | Production method for feather oligopeptide chelating type mineral element |
| CN105661049A (en) * | 2016-03-17 | 2016-06-15 | 上海源耀生物股份有限公司 | Polypeptide copper chelate prepared by using soybean protein isolate as substrate and preparation method |
| CN105967761A (en) * | 2016-05-26 | 2016-09-28 | 陈可夫 | Method for producing amino acid water-soluble fertilizer by utilizing Drawida Japonica Michelsen |
| CN106538844A (en) * | 2016-11-26 | 2017-03-29 | 青岛中泰和生物科技有限公司 | A kind of preparation method of marine protein peptide chelated copper |
| CN106538844B (en) * | 2016-11-26 | 2021-01-01 | 青岛海大生物集团有限公司 | Preparation method of marine organism protein peptide chelated copper |
| CN108218952A (en) * | 2017-12-31 | 2018-06-29 | 连云港大海饲料有限公司 | A kind of preparation method of green feed additive chelating copper ions peptide |
| CN112299930A (en) * | 2020-01-07 | 2021-02-02 | 青岛帝保隆微碳农业技术有限公司 | High-concentration suspended calcium-magnesium fertilizer and preparation method thereof |
| CN112592239A (en) * | 2020-02-06 | 2021-04-02 | 山东世纪瑞文信息技术有限公司 | Seaweed calcium magnesium fertilizer and preparation method thereof |
| CN115215920A (en) * | 2022-07-29 | 2022-10-21 | 重庆工商大学 | Method for preparing small peptide chelated copper by using waste printed circuit board |
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Inventor after: Ma Lizhou Inventor after: Liu Xiangwei Inventor after: Cai Dongmei Inventor after: Zhang Xiaojiao Inventor after: Dong Shuge Inventor after: Sun Peibin Inventor after: Dou Jinhai Inventor before: Ma Lizhou Inventor before: Liu Xiangwei Inventor before: Cai Dongmei Inventor before: Dong Shuge Inventor before: Sun Peibin Inventor before: Dou Jinhai |
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Free format text: CORRECT: INVENTOR; FROM: MA LIZHOU LIU XIANGWEI CAI DONGMEI DONG SHUGE SUN PEIBIN DOU JINHAI TO: MALIZHOU LIU XIANGWEI CAI DONGMEI ZHANG XIAOJIAO DONG SHUGE SUN PEIBIN DOU JINHAI |
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Application publication date: 20121031 |