CN101756041A - Method for preparing casein peptide chelated copper - Google Patents
Method for preparing casein peptide chelated copper Download PDFInfo
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- CN101756041A CN101756041A CN201010040073A CN201010040073A CN101756041A CN 101756041 A CN101756041 A CN 101756041A CN 201010040073 A CN201010040073 A CN 201010040073A CN 201010040073 A CN201010040073 A CN 201010040073A CN 101756041 A CN101756041 A CN 101756041A
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- casein
- enzymolysis liquid
- copper
- peptide chelated
- chelated copper
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Abstract
The invention relates to a method for preparing casein peptide chelated copper, which comprises the following steps of: dissolving casein in deionized water to produce casein suspension; adding protease into the casein suspension to obtain enzymolysis liquid; adding acid into the filtered enzymolysis liquid and adjusting the pH value to 2 to 7; heating the deionized water or distilled water; adding 1/3 to 2/3 enzymolysis liquid into the deionized water or the distilled water and then adding copper sulphate or copper chloride; adding the residual enzymolysis liquid for later use and the copper sulphate or the copper chloride into the mixed liquid to perform chelation reaction; and drying and purifying the reaction liquid to obtain the casein peptide chelated copper. The product obtained by the method has high purity and total production yield. The method has the advantages of simple process and low cost and suitability for scale industrial production.
Description
Technical field
The invention belongs to the additive technology field, be specifically related to a kind of preparation method who in the animal technical field, makes the casein peptide chelated copper of nutriment.
Background technology
Chelate is a kind of compound that obtains organic molecule (amino acid or peptide chain) and metal ion by strong coordinate bond chelating.These compounds are widely used in the animal technical field, because their validity is from the biologically active of related metal, it is used as activator and is used as conditioning agent in the various metabolic functions of all biologic artifacts in the reaction of many enzymes.
Metal ion since with the chelating of the key of peptide chain or amino acid material, help absorption, utilization and the use of metal ion, because it is transported to organic All Ranges by organic component.Especially in the animal technical field, these compounds are used for various raisings or cultivation field to increase and to strengthen normal metabolic and functional activity, and the ability to the output growth of animal has significant positive influences simultaneously.
The chelate that is present at present on the domestic and international market can be divided into all kinds.A most familiar class is and the metal ion kind together that can form complex with specific single amino acids.They are the compound that can fully define on chemical composition, are absorbed by organism easily and utilize.Second class is by forming with the micronutrient that single amino acids forms complex, although this class chelate can not fully define, property class is similar to those of aforesaid kind.In the process of producing these compounds, be also noted that some soluble metal salt is difficult to chelating or stays non-required residual product, as phosphoric acid or hydrochloric acid.The 3rd class includes several, and preferred maximum three kinds of molecular weight the highest 800 daltonian amino acid form the metal ion of complex.But bigger molecular dimension causes bond joint strength more weak and be difficult to more absorb.Last kind be some metal ion can form with some amino acid on the little peptide organic component to the actual nutritional need influence of animal little and metal combine with little peptide must complex, very solvable, and in advocating, be difficult for dissociating, to not influence of pH value in the enteron aisle, can arrive small intestine smoothly, by little intestinal absorption.
Summary of the invention
Purpose of the present invention just provides a kind of preparation method who makes the casein peptide chelated copper of nutriment in the animal technical field, is used for the chelating additive of nutriment, and this additive is not only effective, and it is stable, good water solubility, and produce again easily, and do not have non-required byproduct of reaction.
For realizing this purpose, the inventive method adopts following concrete steps:
(1) casein is dissolved in makes the casein suspension in the deionized water, the weight ratio of casein and deionized water is 1: 2～20 in the casein suspension; PH value with alkali adjusting casein suspension is 7～13 then, and used alkali is NaOH, KOH, NH
3.H
2A kind of among the O.
(2) protease is added the casein suspension, obtain enzymolysis liquid; Contained caseic mass ratio is 1: 30～100 in protease that adds and the casein suspension, 45～65 ℃ of hydrolysis temperatures, enzymolysis time 1～10 hour; Described protease is a kind of in alkali protease, the trypsase or both mixtures.
(3) enzymolysis liquid is filtered, filter out impurities; With the enzymolysis liquid after the acid adding filtration, regulating pH value is 2～7, obtains standby enzymolysis liquid; The acid that adds is HCl or H
2SO
4
(4) in reactor, add deionized water or distilled water, the amount that adds is 3～5 times that standby enzymolysis liquid amasss, be heated to 40～85 ℃, then 1/3～2/3 of standby enzymolysis liquid is joined in deionized water or the distilled water, back adding mantoquita stirs, the amount of the mantoquita that adds was carried out chelatropic reaction in 0.5～2 hour for 5～40%, 40～85 ℃ of following insulated and stirred of the standby enzymolysis liquid weight of adding, obtained elementary chelating liquid; Described mantoquita is copper sulphate or copper chloride.
(5) remaining standby enzymolysis liquid is joined in the elementary chelating liquid, add mantoquita after stirring, the amount of the mantoquita of adding is that 5～40%, 40～85 ℃ of following insulated and stirred of remaining standby enzymolysis liquid weight were carried out chelatropic reaction in 0.5～2 hour, cold filtration after reaction finishes, reactant liquor is stand-by; Described mantoquita is copper sulphate or copper chloride.In whole chelatropic reaction process with HCl or H
2SO
4Regulating pH value is 2～7.
(6) reactant liquor is placed vacuum desiccator be dried to the water weight content below 10%, obtain dry products, the baking temperature of vacuum desiccator is 75～80 ℃; To join in the absolute ethyl alcohol after the dry products pulverizing, stirred 0.5～2 hour, the centrifugal then casein peptide chelated copper sediment that obtains, place vacuum desiccator to be dried to the water weight content sediment below 10%, obtain casein peptide chelated copper, the baking temperature of vacuum desiccator is 75～80 ℃.
Preparation method of the present invention utilizes copper sulphate or copper chloride and the casein hydrolysis peptide characteristic that is insoluble to ethanol soluble in water, when purifying, adopt ethanol to separate out crystallization, obtaining good product purity (content can reach more than 97%) production total recovery is 96%～99%, product is loose uniformly crystal, has good quality.Technology of the present invention is easy, with low cost, and ethanol can recycling, is suitable for large-scale industrial production.
The specific embodiment
Embodiment 1
(1) at first the 400g casein is dissolved in and makes the casein suspension in the 2L deionized water; PH value with NaOH adjusting casein suspension is 13 then.
(2) the 8g alkali protease is added the casein suspension, obtain enzymolysis liquid, hydrolysis temperature is between 55 ℃, and enzymolysis time is 5 hours;
(3) enzymolysis liquid is filtered, filter out impurities; Add H
2SO
4The pH value of regulating enzymolysis liquid is 5, obtains standby enzymolysis liquid.
(4) add deionized water in reactor, the amount of adding is 3 times that standby enzymolysis liquid amasss, is heated to 50 ℃, then 1/3 of standby enzymolysis liquid is joined in the deionized water, and the back that stirs adds CuSO
4, the CuSO of adding
4Amount for 10% of the standby enzymolysis liquid weight that adds, carried out chelatropic reaction in 1 hour 50 ℃ of following insulated and stirred, obtain elementary chelating liquid.
(5) remaining standby enzymolysis liquid is joined in the elementary chelating liquid, the back that stirs adds CuSO
4, the CuSO of adding
4Amount be that 10%, 50 ℃ of following insulated and stirred of remaining standby enzymolysis liquid weight was carried out chelatropic reaction in 1 hour, the reaction back cold filtration that finishes, reactant liquor is stand-by.In whole chelatropic reaction process, use H
2SO
4Regulating pH value is 5.
(6) reactant liquor being placed vacuum desiccator be dried to the water weight content is 8%, obtains dry products, and the baking temperature of vacuum desiccator is 75 ℃; To join in the absolute ethyl alcohol after the dry products pulverizing, stirred 1 hour, the centrifugal then casein peptide chelated copper sediment that obtains, placing vacuum desiccator to be dried to the water weight content sediment is 8%, obtain casein peptide chelated copper, the baking temperature of vacuum desiccator is 75 ℃.
Embodiment 2
(1) at first the 600g casein is dissolved in and makes the casein suspension in the 1.2L deionized water; PH value with KOH adjusting casein suspension is 7 then.
(2) 20g trypsase is added the casein suspension, obtain enzymolysis liquid, hydrolysis temperature is between 65 ℃, and enzymolysis time is 1 hour;
(3) enzymolysis liquid is filtered, filter out impurities; The pH value that adds HCl adjusting enzymolysis liquid is 2, obtains standby enzymolysis liquid.
(4) add deionized water in reactor, the amount of adding is 4 times that standby enzymolysis liquid amasss, is heated to 40 ℃, then 2/3 of standby enzymolysis liquid is joined in the deionized water, and the back that stirs adds CuCl
2, the CuCl of adding
2Amount for 5% of the standby enzymolysis liquid weight that adds, carried out chelatropic reaction in 0.5 hour 40 ℃ of following insulated and stirred, obtain elementary chelating liquid.
(5) remaining standby enzymolysis liquid is joined in the elementary chelating liquid, the back that stirs adds CuCl
2, the CuCl of adding
2Amount be that 5%, 40 ℃ of following insulated and stirred of remaining standby enzymolysis liquid weight was carried out chelatropic reaction in 0.5 hour, the reaction back cold filtration that finishes, reactant liquor is stand-by.Regulating pH value with HCl in whole chelatropic reaction process is 2.
(6) reactant liquor being placed vacuum desiccator be dried to the water weight content is 7%, obtains dry products, and the baking temperature of vacuum desiccator is 80 ℃; To join in the absolute ethyl alcohol after the dry products pulverizing, stirred 0.5 hour, the centrifugal then casein peptide chelated copper sediment that obtains, placing vacuum desiccator to be dried to the water weight content sediment is 7%, obtain casein peptide chelated copper, the baking temperature of vacuum desiccator is 80 ℃.
Embodiment 3
(1) at first the 300g casein is dissolved in and makes the casein suspension in the 6L deionized water; Use NH then
3.H
2The pH value that O regulates the casein suspension is 10.
(2) 2g alkali protease and 1g trypsase are added the casein suspension, obtain enzymolysis liquid, hydrolysis temperature is between 45 ℃, and enzymolysis time is 10 hours;
(3) enzymolysis liquid is filtered, filter out impurities; The pH value that adds HCl adjusting enzymolysis liquid is 7, obtains standby enzymolysis liquid.
(4) add deionized water in reactor, the amount of adding is 5 times that standby enzymolysis liquid amasss, is heated to 85 ℃, then 1/2 of standby enzymolysis liquid is joined in the deionized water, and the back that stirs adds CuCl
2, the CuCl of adding
2Amount for 40% of the standby enzymolysis liquid weight that adds, carried out chelatropic reaction in 2 hours 85 ℃ of following insulated and stirred, obtain elementary chelating liquid.
(5) remaining standby enzymolysis liquid is joined in the elementary chelating liquid, the back that stirs adds CuCl
2, the CuCl of adding
2Amount be that 40%, 85 ℃ of following insulated and stirred of remaining standby enzymolysis liquid weight was carried out chelatropic reaction in 2 hours, the reaction back cold filtration that finishes, reactant liquor is stand-by.Regulating pH value with HCl in whole chelatropic reaction process is 7.
(6) reactant liquor being placed vacuum desiccator be dried to the water weight content is 10%, obtains dry products, and the baking temperature of vacuum desiccator is 78 ℃; To join in the absolute ethyl alcohol after the dry products pulverizing, stirred 2 hours, the centrifugal then casein peptide chelated copper sediment that obtains, placing vacuum desiccator to be dried to the water weight content sediment is 10%, obtain casein peptide chelated copper, the baking temperature of vacuum desiccator is 78 ℃.
Claims (5)
1. the preparation method of a casein peptide chelated copper is characterized in that the concrete steps of this method are:
(1) casein is dissolved in makes the casein suspension in the deionized water, the weight ratio of casein and deionized water is 1: 2～20 in the casein suspension; PH value with alkali adjusting casein suspension is 7～13 then;
(2) protease is added the casein suspension, obtain enzymolysis liquid; Contained caseic mass ratio is 1: 30～100 in protease that adds and the casein suspension, 45～65 ℃ of hydrolysis temperatures, enzymolysis time 1～10 hour;
(3) enzymolysis liquid is filtered, filter out impurities; With the enzymolysis liquid after the acid adding filtration, regulating pH value is 2～7, obtains standby enzymolysis liquid;
(4) in reactor, add deionized water or distilled water, the amount that adds is 3～5 times that standby enzymolysis liquid amasss, be heated to 40～85 ℃, then 1/3～2/3 of standby enzymolysis liquid is joined in deionized water or the distilled water, back adding mantoquita stirs, the amount of the mantoquita that adds was carried out chelatropic reaction in 0.5～2 hour for 5～40%, 40～85 ℃ of following insulated and stirred of the standby enzymolysis liquid weight of adding, obtained elementary chelating liquid;
(5) remaining standby enzymolysis liquid is joined in the elementary chelating liquid, add mantoquita after stirring, the amount of the mantoquita of adding is that 5～40%, 40～85 ℃ of following insulated and stirred of remaining standby enzymolysis liquid weight were carried out chelatropic reaction in 0.5～2 hour, cold filtration after reaction finishes, reactant liquor is stand-by; Regulating pH value with acid in whole chelatropic reaction process is 2～7;
(6) reactant liquor is placed vacuum desiccator be dried to the water weight content below 10%, obtain dry products, the baking temperature of vacuum desiccator is 75～80 ℃; To join in the absolute ethyl alcohol after the dry products pulverizing, stirred 0.5～2 hour, the centrifugal then casein peptide chelated copper sediment that obtains, place vacuum desiccator to be dried to the water weight content sediment below 10%, obtain casein peptide chelated copper, the baking temperature of vacuum desiccator is 75～80 ℃.
2. the preparation method of a kind of casein peptide chelated copper as claimed in claim 1, it is characterized in that: the alkali described in the step (1) is NaOH, KOH, NH
3.H
2A kind of among the O.
3. the preparation method of a kind of casein peptide chelated copper as claimed in claim 1 is characterized in that: the protease described in the step (2) is a kind of in alkali protease, the trypsase or both mixtures.
4. the preparation method of a kind of casein peptide chelated copper as claimed in claim 1 is characterized in that: the acid that adds in step (3) and the step (5) is HCl or H
2SO
4
5. the preparation method of a kind of casein peptide chelated copper as claimed in claim 1, it is characterized in that: the mantoquita described in step (4) and the step (5) is copper sulphate or copper chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010040073A CN101756041A (en) | 2010-01-19 | 2010-01-19 | Method for preparing casein peptide chelated copper |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010040073A CN101756041A (en) | 2010-01-19 | 2010-01-19 | Method for preparing casein peptide chelated copper |
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| Publication Number | Publication Date |
|---|---|
| CN101756041A true CN101756041A (en) | 2010-06-30 |
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|---|---|---|---|
| CN201010040073A Pending CN101756041A (en) | 2010-01-19 | 2010-01-19 | Method for preparing casein peptide chelated copper |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102640857A (en) * | 2012-05-14 | 2012-08-22 | 浙江大学 | Preparation method of rice active peptide chelated copper |
| 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 |
-
2010
- 2010-01-19 CN CN201010040073A patent/CN101756041A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102640857A (en) * | 2012-05-14 | 2012-08-22 | 浙江大学 | Preparation method of rice active peptide chelated copper |
| 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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Application publication date: 20100630 |