CN114354533B - Meat enzymolysis pet food with antioxidant activity and preparation process thereof - Google Patents

Meat enzymolysis pet food with antioxidant activity and preparation process thereof Download PDF

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CN114354533B
CN114354533B CN202210018526.7A CN202210018526A CN114354533B CN 114354533 B CN114354533 B CN 114354533B CN 202210018526 A CN202210018526 A CN 202210018526A CN 114354533 B CN114354533 B CN 114354533B
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杜红星
余璐
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Hongyu Technology Beijing Co ltd
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Abstract

The invention belongs to the field of enzymolysis technology, in particular to meat enzymolysis pet food with antioxidant activity and a preparation technology thereof, comprising the steps of weighing pretreated chicken, adding distilled water according to a material ratio of 1:5, crushing and homogenizing by a crusher, regulating the pH value of a solution to be 4-10, controlling the temperature to be 40-70 ℃, then adding enzyme with the water content of 3-5% to form hydrolysate, adding a controlled release substance and enzyme again in the hydrolysis process, regulating the hydrolysis condition to continue hydrolysis until required supernatant, taking supernatant to prepare powder, and preparing beneficial factors or products comprising pancreatin, chymotrypsin, histidine decarboxylase, selenomethionine, selenium cysteine antioxidant, peptide chain micromolecules for enzymolysis anti-inflammatory and growth-promoting, ascorbyl palmitate, dihydropyridine, astaxanthin, fat, sugar, vitamins, tryptophan, cystine and cysteine by the powder according to the requirement.

Description

Meat enzymolysis pet food with antioxidant activity and preparation process thereof
Technical Field
The invention belongs to the field of enzymolysis technology, and in particular relates to an antioxidant meat enzymolysis pet food and a preparation technology thereof
Background
The peptide amino acid of the protein is only decomposed into required small molecules, which is beneficial to the digestion of pets, and the existing protein decomposition mostly adopts enzymolysis or Maillard reaction, which is also called non-enzymatic browning reaction, and is a non-enzymatic browning widely existing in the food industry. The reaction between carbonyl compound (reducing sugar) and amino compound (amino acid and protein) is carried out, but the technological process is complicated, the reaction process is changeable for pet food, and the enzymatic hydrolysis mainly comprises the steps that protease acts on specific parts in the protein structure to carry out cleavage and decomposition, and the cleavage is decomposed into small molecular peptides or free amino acids. Most animal and microorganism proteins can be subjected to enzymolysis by single enzyme or synergistic action of multiple enzymes, but the enzymolysis is limited in enzyme type and selection of hydrolysis hydrophobic amino acid groups, good cleavage of the hydrophobic groups cannot be finished, and the existing pet food has the defect of slow digestion and quick deterioration, so that the problem of the influence and development of the pet food is needed to be solved.
Disclosure of Invention
In order to achieve at least one of the problems, the invention provides a preparation process of meat enzymolysis pet food with antioxidant activity, comprising weighing pretreated chicken, adding distilled water according to a material ratio of 1:5, crushing and homogenizing by a crusher, adjusting the pH of the solution to 4-10, controlling the temperature to 40-70 ℃, then adding enzyme with the water content of 3-5% to form hydrolysate, adding a controlled release substance and enzyme again during the hydrolysis process, adjusting the hydrolysis condition to continue hydrolysis until the required supernatant, taking the supernatant to prepare powder, and then configuring other nutrition additive substances as required to form the pet food, wherein the enzyme comprises pancreatin and chymotrypsin histidine decarboxylase, so as to improve the effect of cracking hydrophobic groups.
Further, the process of adding the controlled release substances again in the hydrolysis process comprises adding under acidic condition, adding under alkaline condition, or controlling the release of the controlled release substances in the enzymolysis process, wherein the controlled release substances comprise allylthiourea or acrylic acid and salts thereof, and at least one of long-chain alkane or amino acid or long-chain pyridine or amino residue pyridine is selected to react to form the controlled release substances.
Further, the measurement and control substance comprises acrylic acid, allylthiourea and selenomethionine, or the measurement and control substance comprises allylthiourea, acrylic acid and long-chain alkene pyridine which comprises a magnesium histidine residue substance containing pyridine and a hydrocarbon alkyl methionine ester substance
Figure BDA0003461562270000021
Further, the preparation process of the controlled release material comprises the following steps of mixing acrylic acid, allylthiourea and selenomethionine according to a mass ratio of 20:3: adding 1 into aqueous solution, adding 3:1 private plate 60 and Tween 60 in mass ratio of 1.2 times of kerosene, adding the aqueous solution into the kerosene, stirring into emulsion, and when the catalytic reaction of deoxidizing and adding ammonium persulfate is not exothermic, forming polymeric polymer emulsion, taking an emulsion sample for electron microscope observation, demulsifying the emulsion after the reaction, drying and constant weight crushing the viscous substance after demulsifying, preparing an aqueous solution of the crushed substance, and testing viscosity and molecular weight by using a capillary tube to be favorable for keeping the filtering particle size.
Further, the preparation of the substance containing the structural formula I comprises the preparation process of the substance containing pyridine histidine magnesium residue and the preparation process of the substance containing hydrocarbon alkyl methionine ester,
the first step: preparing a pyridine-containing magnesium histidine residue substance, preparing a 3% magnesium chloride solution, regulating pH to 6.9-9, adding 3-10g of ammonium carbonate into the solution to precipitate, adding histidine at a low temperature until the precipitate is dissolved, testing the pH of a supernatant to be 6-7, adding N, N' -diisopropylcarbodiimide and dichloromethane, then sequentially adding 5-vinyl pyridine formate for heating reaction, and testing the pyridine-containing magnesium histidine residue contained in the formed substance after the separation treatment of a reaction solution;
and a second step of: preparation of hydrocarbon-containing alkyl methionine ester material: selenomethionine and N- (5-chloro-2, 4-dimethoxy phenyl) -3-hydroxy-2-naphthamide are mixed and then dicyclohexylcarbodiimide is added at low temperature, then 4-dimethylamine pyridine is prepared into a solution and added drop by drop until the reaction heat release is stopped, solid-liquid separation and purification are carried out, a 1:1 solution is prepared by using a purified substance, and a small amount of purified solution is taken to test the formation of the substance containing ester groups;
and a third step of: adding a magnesium histidine residue substance containing pyridine and a hydrocarbon alkyl methionine ester substance into a solution containing ethanol acetone according to a mass ratio of 5:1, wherein the ratio of the hydrocarbon alkyl methionine ester substance is preferably 10:1 so that the ratio of the hydrocarbon alkyl methionine ester substance is small, heating and refluxing under nitrogen sealing to react to form a solution into paste, distilling under reduced pressure to remove a solvent to form a controlled release substance containing a component of a structural formula I, and mixing acrylic acid, allylthiourea and the controlled release substance containing the component of the structural formula I according to a mass ratio of 20:3:0.3 is added into aqueous solution containing formamide, and the emulsification reaction is carried out under the condition of 40-80 ℃ to generate the controlled release material with the structural formula I.
Further, the basic performance test method comprises the following steps of: firstly, taking a measurement and control release substance as a substance for testing copper ion catalytic decomposition property, weighing distilled water, putting the distilled water into the same glass beaker SB1 and glass beaker SB2, adding copper oxide with different amounts into the glass beaker SB1 and the glass beaker SB2, then regulating the pH of the solution in each beaker, controlling the temperature to be 40-60 ℃, then hydrolyzing the solution for several hours according to the equal weight parts of pancreatin, chymotrypsin and histidine decarboxylase with the water content of 3-5% to form a hydrolysate, taking the supernatant of the hydrolysate in the beaker, respectively adding the measurement and control release substance with a certain concentration, regulating the pH after the supernatant is hydrolyzed for several hours again, respectively taking a certain amount of supernatant of the SB1 and the SB2, respectively filtering the supernatant with filter papers with the pore diameters not exceeding a certain size, taking the weight of the filtrate, and judging degradation conditions according to the recovery rate of supernatant filtration;
filtering supernatant of SB1 and SB2 respectively, dewatering with ethanol, cleaning, oven drying filtrate to constant weight, recording as XNSB1 and XNSB2 samples, preparing deionized water solution with certain concentration from XNSB1 and XNSB2, measuring viscosity value as XNSB1N, XNSB N after converting with capillary test viscosity N, calculating molecular weight of XNSB1 and XNSB2 as XNSB1FXNSB2F,
secondly, taking a certain number of XNSB1 and XNSB2 samples, putting the samples into a muffle furnace, burning the samples to constant weight at a certain temperature, taking the samples out, cooling the samples to room temperature, respectively adding sulfuric acid solution for dissolving the samples, adjusting pH to obtain a certain amount of neutral solution, respectively adding a certain amount of ammonia water into the solution to generate blue color, and testing the chromaticity C value of the solution by using a handheld intelligent colorimeter, wherein the chromaticity value is XNSB1CD and XNSB2CD;
and finally, comparing and testing, namely simulating the existence of copper ions in an animal body, preparing a reference quantity containing copper ions with a certain concentration, adding sulfuric acid solution for dissolving, regulating pH value, processing into a certain quantity of neutral solution, respectively generating blue color to a certain quantity of ammonia water in the solution, testing the value of chromaticity CD by using a handheld intelligent colorimeter, comparing and testing to show the quantity and existence state of the copper ions, and judging whether the enzymolysis reaction generates the copper ions in an out-of-standard decomposition state or not according to the molecular weight or the condition of the enzymolysis reaction or the molecular weight according to a corresponding parameter formula by combining the filtration recovery rate of the supernatant fluid of the controlled release substance in the basic performance test with the molecular weight and viscosity of the controlled release substance obtained in the basic performance test.
Further, the method comprises the steps of judging and regulating enzymolysis reaction according to test data after the measurement and control release substances participate in the enzymolysis process:
and judging the protein decomposition condition by using the recovery rate of the supernatant fluid filtrate after the measurement and control release substances participate in the enzymolysis process, and then combining the viscosity value after the measurement and control release substances participate in the enzymolysis process, wherein the molecular weight judgment after the measurement and control release substances participate in the enzymolysis process comprises the ionic state condition of copper in the enzymolysis process or the condition of the measurement and control enzymolysis process.
Further, the method for testing the state of copper ions in enzymolysis by using the controlled release substance comprises the following steps: weighing pretreated meat and animal viscera, performing enzymolysis by using part of processes in the preparation process of the meat enzymolysis pet food with antioxidant activity, wherein the part of processes comprises adjusting the pH value of a solution to 4.5, controlling the temperature to 60 ℃, hydrolyzing with 3% of pancreatin, chymotrypsin and histidine decarboxylase in equal parts by weight for 1h to form hydrolysate, adding 0.05% of a release-measuring substance XN into supernatant of the hydrolysate to hydrolyze for 0.5h, adjusting ph to 8 to hydrolyze for 0.5h, taking 100g of supernatant, filtering with filter paper with a pore diameter of not more than 1um, carrying out weight measurement on the filtrate, calculating the recovery value XNSBHS of the supernatant filtrate, judging the proteolytic condition of chicken according to the recovery value XNSBHS, taking the filtered filter paper to dehydrate and wash with ethanol, recording the filtrate with constant weight as XNSB, preparing a 0.3 deionized water solution of XNSB, converting the viscosity value into XNSBN, calculating the molecular weight, and judging according to the following: when the molecular weight of XN is less than 200 ten thousand and the supernatant filtering recovery rate is more than 93.6%, the XN molecules are degraded too quickly; when the molecular weight of XN is more than 226 ten thousand and the filtering recovery rate of supernatant is less than 93.6%, the degradation of XN molecules is in a basic range;
further, a method for measuring and controlling the enzymolysis process of the measuring and controlling release substances comprises the steps of selecting a certain amount of supernatant, adding a certain amount of phosphatidylcholine, stirring uniformly, testing, and judging conditions including control of copper, control of magnesium or control of amino acid in the enzymolysis process according to conditions of recovery rate and viscosity value change of filtrate of the measuring and controlling release substances in the enzymolysis process, namely XN2, in the method for measuring and controlling the copper ion state in the enzymolysis by using the measuring and controlling release substances, drying and constant weight of the filtrate after XN2 filtration and testing, recording as XN2SB, taking the XN2SB for infrared spectrum test, and concentrating the supernatant after the enzymolysis of the measuring and controlling release substances in the basic performance test method of the measuring and controlling release substances.
The invention also provides meat enzymolysis pet food with antioxidant activity, which comprises beneficial products, ascorbyl palmitate, dihydropyridine, astaxanthin, fat, saccharides, vitamins, tryptophan, cystine and cysteine which appear after the measurement and control release substance participates in the enzymolysis process.
The invention has the beneficial effects that: the method has the advantages that the cracking of hydrophobic groups is improved, the decomposition is prevented, the optimization of the anti-infection digestion-aiding effect of pet food is assisted, the rapid development effect is improved, the pet food has the multiplying power for the growth and development of pets compared with the common pet food, the quality guarantee period and the oxidation resistance of the pet food produced by different measurement and control release processes are improved by at least about half a year compared with the common pet food, the method is high in applicability and good in popularization, the method further has the effect of adjusting enzymolysis and adjusting correspondingly to measurement and control release, and the measurement and control release substances in the integral structure further have the effect of controlling release regulators synchronously with ions.
Drawings
Fig. 1: electron microscope image for measuring and controlling the state of the emulsion of the releasing substance;
fig. 2: making an infrared detection spectrum of a measurement and control release substance containing a structural formula I;
fig. 3: and measuring and controlling infrared spectrogram of XN2SB of the filtered matter after the filtering test of XN 2.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
A process for preparing the antioxidizing active meat-type food for pet includes such steps as proportionally mixing pretreated meat, animal viscera, chicken and chicken viscera, adding distilled water or alcohol-contained organic solution at 1:5, high-speed pulverizing, homogenizing, regulating pH to 4-10, controlling temp to 40-70 deg.C, adding enzyme 3-5% of water to obtain hydrolytic liquid, adding the substances and enzyme for controlling hydrolysis, regulating the hydrolytic condition, hydrolyzing, pulverizing, adding nutritive additives, and preparing the enzyme including pancreatin, chymotrypsin histidine decarboxylase.
The process of adding the controlled release substances again comprises the process of adding the controlled release substances under an acidic condition or adding the controlled release substances under an alkaline condition or releasing the controlled release substances after enzymolysis reaction or releasing the controlled release substances after the addition or releasing the controlled release substances to another hydrolysis section after the addition, and the like, wherein the controlled release substances comprise at least one of allylthiourea or acrylic acid and salts thereof, selected long-chain alkane or amino acid or long-chain pyridine or amino residue pyridine, and the like, for example, sodium acrylate is formed by reacting with amino acid, for example, allylthiourea, acrylic acid and long-chain alkane, so as to realize the control of transition metals including copper, and further regulate the enzymolysis and the controlled release substances.
The measurement and control substance comprises acrylic acid, allylthiourea and selenomethionine, or the measurement and control substance allylthiourea, and the acrylic acid and long-chain alkene pyridine react to generate a substance containing a structural formula I, wherein the long-chain alkene pyridine comprises a pyridine-containing magnesium histidine residue substance and a hydrocarbon-containing alkyl methionine ester substance, the long-chain pyridine comprises a long-chain alkyl-containing pyridine, the residue pyridine comprises a pyridine-containing magnesium histidine residue, the long-chain alkene pyridine-containing substance further comprises a substance matched with a phosphatidylcholine component,
the following describes the process for preparing the controlled release material XN
The measurement and control substances comprise the preparation of substances generated by the reaction of acrylic acid, allylthiourea and selenomethionine, wherein the mass ratio of the acrylic acid to the allylthiourea to the selenomethionine is (20:3): adding 1 into aqueous solution, adding 3:1 private plate 60 and Tween 60 in mass ratio of 1.2 times of kerosene, adding the aqueous solution into kerosene, stirring to form emulsion, and adding oxygen to the aqueous solution to form polymer emulsion when the catalytic reaction of ammonium persulfate is not exothermic, taking an emulsion sample for electron microscopy, wherein the particle size of the emulsion is more than 1200nm as shown in an electron microscopy image 1, demulsifying the reacted emulsion, drying and constantly weighing the demulsifying sticky substances, crushing the demulsifying sticky substances to obtain a controlled release substance XN1, preparing 0.3% XN1 solution by using ion water, converting the viscosity value of 9mpa.s by using capillary test viscosity N, calculating about 230 ten thousand of molecular weight, and controlling the state of the controlled preferred molecular weight of 200 ten thousand, so that the filter particle size is favorable for maintaining.
Further, the measurement and control substance allyl thiourea, acrylic acid and long-chain alkyl olefin pyridine react to generate a substance containing the following structural formula I, or comprises the preparation of a substance containing pyridine histidine magnesium residue and the preparation of a substance containing hydrocarbon alkyl methionine ester,
specifically, the first step: preparing a pyridine-containing magnesium histidine residue substance, preparing a 3% magnesium chloride solution, regulating and matching pH to 6.9-9 to precipitate, adding 3-10g of ammonium carbonate into the solution, then adding histidine at a low temperature of 15-40 ℃ until the precipitate is dissolved, and further, measuring pH of a supernatant to be 6-7, keeping pH of the supernatant at 7.1-9, adding a magnesium reagent to change color obviously, regulating pH to 9.5, generating blue turbidity, indicating that the reaction forms magnesium ion carboxylic acid group complexation by acid-base change and salt color change, also proving amino positive ions under the conditions, titrating by a general EDTA method, generating red color, observing turbidity to further prove that the stability of different carboxyl complexation and different complexation in different pH is different, and indicating that magnesium histidine is formed; dropwise adding acid into the supernatant to release gas to indicate that magnesium carbonate exists, then adding 5-vinyl pyridine formate into the supernatant to carry out heating reaction under the conditions of dehydration of N, N' -diisopropylcarbodiimide and methylene dichloride solvent, separating reaction liquid, heating the supernatant to remove unreacted magnesium carbonate influence, adding a small amount of dried substance into solution, adding magnesium reagent I into the solution to carry out reaction for a few minutes, adding ammonia monohydrate again, heating to generate mauve, and testing histidine magnesium residues possibly formed and containing pyridine;
and a second step of: preparation of hydrocarbon-containing alkyl methionine ester material: selenomethionine, N- (5-chloro-2, 4-dimethoxyphenyl) -3-hydroxy-2-naphthoamide can be mixed into a soluble solution, DCC (dicyclohexylcarbodiimide) is added at low temperature, DMAP (4-dimethylaminopyridine) is prepared into a solution, the solution is slowly added drop by drop, after the reaction exotherm is stopped, solid-liquid separation and purification are carried out, a 1:1 solution is prepared by using a purified substance, a small amount of the purified solution is added into an acidic phenolphthalein solution to be colorless, the solution is heated to appear red, and the existence of ester groups is determined, further, when needed, the basic protection, such as esterification reaction under the action of DCC/DMAP by using Boc protective amino groups, the product is obtained after the reaction is removed and protected by trifluoroacetic acid, and further, other matchable hydrophobic substances such as di (hydroxyethyl) methyldodecylammonium chloride or 6-chloro-2-hydroxyaniline can be selected to replace N- (5-chloro-2, 4-dimethoxyphenyl) -3-hydroxy-2-naphthoamide;
and a third step of: adding a magnesium histidine residue substance containing pyridine and a hydrocarbon alkyl methionine ester substance into a solution containing ethanol acetone according to a mass ratio of 5:1, heating and refluxing under the airtight regulation of nitrogen to react to form a paste, distilling under reduced pressure to remove a solvent to form a controlled release substance containing a component of a structural formula I, and adding acrylic acid, allylthiourea and the controlled release substance containing the component of the structural formula I according to a mass ratio of 20:3:0.3 is added into aqueous solution containing formamide, and the measurement and control substance XN1 is prepared in the same time under the condition of 40-80 ℃ in the way of emulsification reaction to generate the measurement and control substance with the structural formula I
Figure BDA0003461562270000101
The infrared detection spectrum of the measurement and control release substance containing the structural formula I is shown in the figure, the peak type weak instruction olefin double bond at 1600cm < -1 > is basically opened, the characteristic absorption of carboxyl groups at 3500cm < -1 >, 2690cm < -1 >, 1690cm < -1 > is the existence of acrylic acid, the strong peak in 1110cm < -1 >, the thin and weak peak at about 700 and 800cm < -1 > are the characteristic absorption of histidine, the characteristic absorption of N substituted pyridine at 1540, the thiourea peak appears at 900-1300cm < -1 >, the amino absorption peak of 3530-3280 cm < -1 > methionine, the hydroxyl absorption peak at 3600cm < -1 >, the characteristic peak of N- (5-chloro-2, 4-dimethoxy phenyl) -3-hydroxyl-2-naphthamide at about 2900cm < -1 >, and the like are also shown in the figure. It is understood that the substance containing the structural formula I can produce long-chain alkyl olefin pyridine, and the formation of the corresponding substances in the preparation process of the controlled release substance is also illustrated in the form of images, and the substance containing the magnesium histidine residue of pyridine and the substance containing hydrocarbon alkyl methionine ester can be independently matched for use.
Fourthly, preparing a measurement and control release substance XN2, wherein the preparation is different from XN1 on the basis of XN1 in that acrylic acid, allylthiourea and the measurement and control release substance containing a component with a structural formula I are formed according to a mass ratio of 20:3:0.3 is added into aqueous solution containing formamide to react under the condition of 40-80 ℃ to generate XN2, an emulsion sample is taken for electron microscopy, the electron microscopy data can be known as 1100nm, 0.3% of XN2 is prepared into an ionic aqueous solution, the viscosity value is 7mpa.s after the conversion of capillary test viscosity N, the calculated molecular weight is about 228 ten thousand, the characteristic is that the test viscosity becomes 10mpa.s after 0.1% of phosphatidylcholine or 0.01% K12 is added into 0.3% of XN2 substance solution, the capillary test molecular weight is 229 ten thousand, the viscosity becomes larger without changing the molecular weight, the principle of the viscosity change is that the phosphatidylcholine is physically associated with long-chain alkyl and pyridine ring molecules, the viscosity change caused by the physical change is not changed, and the effect is beneficial to the control output and the test of enzymolysis reaction substances, such as the viscosity change is beneficial to be added and the safe filtration separation is carried out.
The following illustrates a basic performance test method of a copper ion catalytic measurement and control release substance XN
Firstly, taking XN1 as copper ion catalytic decomposition test, weighing distilled water, putting into a glass beaker SB1 and a glass beaker SB2 which are the same, adding 10mg/kg of copper oxide into SB1, adding 100mg/kg of copper oxide into SB2, regulating the pH of the solution to 4.5 in each beaker, controlling the temperature to 60 ℃, hydrolyzing 1h according to 3% of added pancreatin, chymotrypsin and histidine decarboxylase in equal weight parts to form hydrolysate, respectively adding 0.05% XN1 into the supernatants of the two beakers for 0.5h, regulating ph to 8 for 0.5h, respectively taking 100g of SB1 and SB2 supernatant, respectively filtering with filter paper with the aperture of not more than 1um, carrying out the weighing of the filtrate, wherein the filtering weight of SB1 supernatant is 93.6g, the filtering weight of the SB2 supernatant is 93.7, the recovering rate of HS 1 of the SB1 is 93.6%, the recovering rate of HS of SB2 supernatant is 93.7%, and the recovering rate of the HS of the SB2 is 83+3, respectively filtering the supernatant of the SB2 is less than 1000nm, and the supernatant of the supernatant can be degraded to be less than 1000nm under the conditions of no degradation of XN1 and no degradation of the XN1 is shown in the beakers;
then, respectively taking filter papers after filtering SB1 and SB2 supernatant fluid, dehydrating and cleaning the filter papers by ethanol, drying the filter materials to constant weight, marking the filter materials as XN1SB1 and XN1SB2, taking XN1SB1 and XN1SB2 to prepare 0.3 deionized water solution, converting the solution into a capillary test viscosity N to obtain viscosity values of XN1SB1N of 8.9mpa.s and XN1SB2N of 6mpa.s, calculating that the molecular weight values of XN1SB1 and XN1SB2 are respectively 226 ten thousand and XN1SB2F of 132 ten thousand, taking 10g of XN1SB1 and XN1SB2 sample, putting the sample into a muffle furnace to burn to constant weight at 500 ℃, taking out and cooling to room temperature, respectively adding sulfuric acid solution to dissolve, adjusting pH to neutral solution to 10g, respectively adding 0.5g of ammonia water into the solution to generate blue color, testing the chromaticity values of XN1SB1CD and XN1SB2CD of 0.05 DEG and 0.43 DEG respectively by using a handheld intelligent colorimeter,
finally, comparing and testing, namely preparing a reference quantity for simulating the existence of copper ions in an animal body, namely preparing 10mg/kg copper ions, adding 10g of solution with neutral pH after dissolving in sulfuric acid solution, respectively adding 0.5g of ammonia water into the solution to generate blue color, testing the value of chromaticity CD to be 0.052 ℃ by using a handheld intelligent colorimeter, and basically approaching to the value of the end CD under the corresponding condition to 0.05 ℃, wherein the comparing and testing shows that the regression accuracy of test data is higher, and also proves that copper exists as ions, the combination of a controlled release substance to copper, the existence quantity of copper ions and the influence of copper ions on the degradation of the controlled release substance in the environment are also verified.
From the above, the filtering recovery rate of the supernatant of the XN1 substance under the above scheme conditions can influence the molecular weight and viscosity of the XN1 substance, so as to rapidly judge whether the enzymolysis reaction of the invention generates the copper ions in the over-standard decomposition state, and when the molecular weight of the XN is less than 200 ten thousand and the filtering recovery rate of the supernatant is more than 93.6%, the existence of the excessive rapid degradation of the XN molecules is indicated, and the existence of more copper in the ion state is indicated. When the molecular weight of XN is more than 226 ten thousand and the filtering recovery rate of supernatant is less than 93.6%, the degradation of XN molecules is in a basic range;
further, it is explained that there may be a decomposition of CuPZn-SOD by histidine decarboxylase, and the situation of fragment ion content is judged. Further, the control conditions and the enzymolysis reaction conditions of the ions including copper under the above conditions can be judged according to the molecular weight and the viscosity of XN1, further, the data is analyzed, the conversion of the combination percentage quantity can be known, the approximate linear relation between the molecular weight and the viscosity of XN1 and the control conditions of copper ions under the above scheme is obtained, the combination test evaluates the influence of the copper ions on the molecular weight and the viscosity under the above conditions, and when the filtration recovery rate of XN1 substance supernatant is less than 93.6% and the molecular weight is more than 200, the data range M= (44 XN1SB 1N/89) + (28 XN1 SBF/113) of the control values of copper ions under the above conditions is preferably pre-judged according to the following formula, so as to realize the judgment of the molecular weight or the judgment of the enzymolysis conditions or the judgment of the molecular weight according to the corresponding parameter formula.
The following description is made of judging the protein decomposition condition according to the condition that the measurement and control release substance XN participates in the enzymolysis process, and judging the ionic state condition of copper in the enzymolysis process or the condition that the measurement and control of the enzymolysis process is performed according to the molecular parameters including the molecular weight after the substance XN participates in the enzymolysis process, such as whether the proteolysis of the enzymolysis process is complete or not, by combining the viscosity value after the substance XN participates in the enzymolysis process.
The method specifically comprises the following steps of preferably testing the state of copper ions in enzymolysis by a substance XN 1: weighing pretreated meat and animal viscera, preferably meat of broiler, purchasing in a supermarket, adding distilled water according to a material ratio of 1:5, crushing and homogenizing by a high-speed crushing homogenizer, regulating the pH value of the solution to 4.5, controlling the temperature to 60 ℃, adding the following pancreatin, chymotrypsin and histidine decarboxylase in the proportion of 3% of the added water, hydrolyzing for 1h to form hydrolysate, adding 0.05% XN1 into supernatant of the hydrolysate to hydrolyze for 0.5h, regulating ph to 8 to hydrolyze for 0.5h, taking 100g of supernatant, filtering by filter paper with the aperture of not more than 1um, weighing 89.2g of filtrate, recovering XN1SBHS to 90.3%, considering filtering loss, recovering rate to 93, indicating that most chicken is thoroughly hydrolyzed by ethanol, drying and cleaning the filtered filter paper, recording the dried and constant weight as XN1SB, taking XN1SB to prepare 0.3 deionized water solution, obtaining viscosity value as XN 1N as 8.6mpa.s after conversion by capillary test viscosity N, calculating the molecular weight of the substances in the sample to be about 212: when the molecular weight of XN is less than 200 ten thousand and the supernatant filtration recovery rate is more than 93.6%, the existence of excessive rapid degradation of XN molecules indicates that more copper exists in an ionic state, and the histidine decarboxylase hydrolysis can be strong. When the molecular weight of XN is more than 226 ten thousand and the filtering recovery rate of supernatant is less than 93.6%, the degradation of XN molecules is in a basic range; from this, it is known that slightly more ionic copper is present in the enzymatic hydrolysis process, and that the decomposition of CuPZn-SOD by histidine decarboxylase may cause the rapid oxidation of the process.
The method comprises the steps of testing the state of copper ions in enzymolysis by using a substance XN2 or measuring and controlling the condition of the enzymolysis process: on the basis of the test method for measuring and controlling the release of the substance XN1 under the same condition, the method is different from the test of the substance XN1 in that 100g of supernatant can be selected, 0.1 percent of phosphatidylcholine is added for uniformly stirring and testing, the following data are obtained by testing under the action of no phosphatidylcholine, the recovery rate XN2SBHS of the filtrate of the substance XN2 is 89.7 percent by the test method of the substance XN1, the viscosity value of the substance XN2 after participating in the enzymolysis process is 6.5mpa.s, the molecular weight of the substance XN2 after participating in the enzymolysis process is about 220 ten thousand,
from the above data, it is known that the recovery rate of the filtrate of the material XN2 is reduced in the enzymolysis process, the viscosity value of the material XN2 after participating in the enzymolysis process is smaller, there is a possibility that the proteolysis is incomplete, the viscosity and molecular weight change are smaller, which indicates the existence of copper ions, further indicates that but does not reach the corresponding result when testing the material XN1, the hydrolysis of histidine decarboxylase is weak, thus according to the above data, the filtrate of the material XN2 after the filtration test in the above test is dried to constant weight and then is recorded as XN2SB, XN2SB is taken for infrared spectrum test, the infrared spectrum shows that the characteristic peak of pyridine, the characteristic peak of N- (5-chloro-2, 4-dimethoxyphenyl) -3-hydroxy-2-naphthamide, the carboxyl and thiourea appear, in particular, the peak of copper complex appears between 300 and 600cm-1, the strong peak in 1110cm-1, the weak histidine peak at about 700 and 800cm-1 and the correlation peak of methionine at 3530 to 3280cm-1 are not obvious, which indicates that no histidine magnesium residue appears, no selenomethionine appears, which indicates that at least chymotrypsin does not cleave hydrophobic groups such as alkylpyridine, the molecular structure and the corresponding cationic group have the function of resisting cleavage of chymotrypsin in the enzymolysis environment, after XN1 is converted into XN2 in the basic performance test method of XN, supernatant liquid is taken for concentration detection, the presence of magnesium ions, the deletion of histidine magnesium residue and the appearance of magnesium indicate that histidine decarboxylase acts, the control of copper and the control of magnesium and amino acid exist, further, it is explained that the decomposition and control of histidine groups under the condition of resistance, the subsequent hydrolysis of histidine decarboxylase may be weak or the molecular parameters or structures including hydrophobic hydrocarbon amine groups are inhibited after the release of amino acids in the molecular structure, so as to reduce the performance of histidine decarboxylase, and in addition, the preparation test method and the use process and the principle of the scheme of the invention are consistent with those of N- (5-chloro-2, 4-dimethoxyphenyl) -3-hydroxy-2-naphthoamide after replacing N- (5-chloro-2, 4-dimethoxyphenyl) -3-hydroxy-2-naphthoamide with bis (hydroxyethyl) methyl dodecyl ammonium chloride or 6-chloro-2-hydroxyaniline.
The analysis of the results shows that the use of the controlled release material XN2 in the enzymolysis scheme is that the controlled release material XN2 is added in the later stage of the pH4.5 stage, which is beneficial to the control of the enzymolysis to be thoroughly carried out. Furthermore, the XN2 substance is added or automatically released under alkaline condition to have the effect of controlling the adsorption of polar amino acid, and further the detection of enzymes such as histidine decarboxylation and the like on SOD decomposition is further combined with the control of copper ions, and the control of magnesium ions is also beneficial to evaluating the performance of methionine adenylate transferase. The invention relates to a method for testing change by adding phosphatidylcholine or K12 into a solution of a certain amount of a release-controlling substance XN 2.
In addition, the application example of the invention is fed with the actual feeding and eating result feedback, and the pet food produced after different measurement and control release substances are added in the process of the invention, for example, the pet food prepared according to relevant standard quantity after the measurement and control release substances are not needed to be separated after the measurement and control release substances are added in the enzymolysis process comprises selenomethionine, tryptophan and selenium cysteine antioxidant substances, peptide chain micromolecules, anti-inflammatory health care and development promoting beneficial factors or products generated by enzymolysis, ascorbyl palmitate, dihydropyridine, astaxanthin, fat, saccharides, vitamins, tryptophan, cystine and cysteine, and the pet food fed by the invention is compared with the common pet food and the common experimental condition under the same condition, the growth and development speed of the pet food prepared by the measurement and control release substances XN1 in the process is improved by 0.3 times compared with the common pet food, the growth and development speed of the common pet food prepared by the measurement and control release substances XN2 in the process is improved by 0.5 times, and the anti-oxidation performance period of the pet food produced by the invention is improved by the invention by the process of adding different pet foods and the oxidation resistance of the pet food and the quality guarantee period of the pet food is improved by 0.6 years compared with the common pet food.
The invention belongs to the field of enzymolysis technology, in particular to an antioxidative meat enzymolysis pet food and a preparation technology thereof, comprising the steps of weighing pretreated chicken, adding distilled water according to a material ratio of 1:5, crushing and homogenizing by a crusher, regulating the pH value of a solution to be 4-10, controlling the temperature to be 40-70 ℃, then adding enzymes with the water content of 3-5% to form hydrolysate, adding measurement and control substances and enzymes again in the hydrolysis process, regulating hydrolysis conditions to continue hydrolysis until required supernatant liquid is obtained, taking supernatant liquid to prepare powder, and then carrying out enzymolysis on the pet food according to the requirements.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (6)

1. A preparation process of meat enzymolysis pet food with antioxidant activity comprises weighing pretreated chicken, adding distilled water according to a material ratio of 1:5, pulverizing and homogenizing with a pulverizer, adjusting pH of the solution to 4-10, controlling temperature to 40-70deg.C, and adding enzyme with water content of 3-5% to form hydrolysate, and is characterized in that: adding a measurement and control release substance and enzyme again in the hydrolysis process, regulating the hydrolysis condition, continuing to hydrolyze to the required supernatant, taking the supernatant for milling, and then preparing other nutrition additive substances as required to form pet food, wherein the enzyme comprises pancreatin or chymotrypsin or histidine decarboxylase so as to improve the effect of splitting hydrophobic groups;
the process of adding the controlled release substances again in the hydrolysis process comprises adding under an acidic condition, adding under an alkaline condition, or controlling the release of the controlled release substances in the enzymolysis process, wherein the controlled release substances comprise allylthiourea or acrylic acid and salts thereof, and the controlled release substances are formed by selecting at least one of long-chain alkane or amino acid or long-chain pyridine or amino residue pyridine for reaction;
the controlled release substances comprise acrylic acid, allylthiourea and selenomethionine, or the controlled release substances comprise allylthiourea, acrylic acid and long-chain alkene pyridine which comprises magnesium histidine residue substances containing pyridine and substances containing hydrocarbon alkyl methionine ester
Figure QLYQS_1
The preparation process of the controlled release substance comprises the following steps:
acrylic acid, allylthiourea and selenomethionine are mixed according to the mass ratio of 20:3: adding 1 into aqueous solution, adding span 60 and Tween 60 in a mass ratio of 3:1 into kerosene of 1.2 times, adding the aqueous solution into kerosene, stirring to form emulsion, removing oxygen, adding ammonium persulfate, catalyzing and reacting, forming polymer emulsion when heat is not released, taking emulsion sample, performing electron microscope observation, demulsifying the emulsion after the reaction, drying and constant weight crushing the viscous substance after demulsifying, preparing an aqueous solution of crushed substance, and testing viscosity and molecular weight by using a capillary tube to be beneficial to keeping the filtering particle size.
2. The process for preparing an antioxidative meat-based enzymatic pet food comprising the steps of: the preparation of substances containing structural formula I comprises the preparation of substances containing pyridine histidine magnesium residues and the preparation of substances containing hydrocarbon alkyl methionine esters;
the first step: preparing a pyridine-containing magnesium histidine residue substance, preparing a 3% magnesium chloride solution, regulating pH to 6.9-9, adding 3-10g of ammonium carbonate into the solution to precipitate, adding histidine at a low temperature until the precipitate is dissolved, testing the pH of a supernatant to be 6-7, adding N, N' -diisopropylcarbodiimide and dichloromethane, then sequentially adding 5-vinyl pyridine formate for heating reaction, and testing the pyridine-containing magnesium histidine residue contained in the formed substance after the separation treatment of a reaction solution;
and a second step of: preparation of hydrocarbon-containing alkyl methionine ester material: selenomethionine and N- (5-chloro-2, 4-dimethoxy phenyl) -3-hydroxy-2-naphthamide are mixed and then dicyclohexylcarbodiimide is added at low temperature, then 4-dimethylamine pyridine is prepared into a solution and added drop by drop until the reaction heat release is stopped, solid-liquid separation and purification are carried out, a 1:1 solution is prepared by using a purified substance, and a small amount of purified solution is taken to test the formation of the substance containing ester groups;
and a third step of: adding a magnesium histidine residue substance containing pyridine and a hydrocarbon alkyl methionine ester substance into a solution containing ethanol acetone according to a mass ratio of 5:1, heating and refluxing under nitrogen sealing to react to form a paste, distilling under reduced pressure to remove a solvent to form a controlled release substance containing a component of a structural formula I, and mixing acrylic acid, allylthiourea and the controlled release substance containing the component of the structural formula I according to a mass ratio of 20:3:0.3 is added into aqueous solution containing formamide, and the emulsification reaction is carried out under the condition of 40-80 ℃ to generate the controlled release material with the structural formula I.
3. The process for preparing the meat-based enzymatically active pet food having antioxidant activity of claim 2, wherein: the basic performance test method comprises the following steps of: firstly, taking a measurement and control release substance as a substance for testing copper ion catalytic decomposition property, weighing distilled water, putting the distilled water into the same glass beaker SB1 and glass beaker SB2, adding copper oxide with different amounts into the glass beaker SB1 and the glass beaker SB2, then regulating the pH of the solution in each beaker, controlling the temperature to be 40-60 ℃, then hydrolyzing the solution for several hours according to the equal weight parts of pancreatin, chymotrypsin and histidine decarboxylase with the water content of 3-5% to form a hydrolysate, taking the supernatant of the hydrolysate in the beaker, respectively adding the measurement and control release substance with a certain concentration, regulating the pH after the supernatant is hydrolyzed for several hours again, respectively taking a certain amount of supernatant of the SB1 and the SB2, respectively filtering the supernatant with filter papers with the pore diameters not exceeding a certain size, taking the weight of the filtrate, and judging degradation conditions according to the recovery rate of supernatant filtration;
filtering supernatant fluid of SB1 and SB2 respectively, dehydrating and cleaning filter paper with ethanol, drying the filtrate to constant weight, marking the filtrate as XNSB1 and XNSB2 samples, preparing deionized water solution with certain concentration by XNSB1 and XNSB2, obtaining viscosity values which are respectively calculated as XNSB1N, XNSB N after converting the viscosity N by capillary test, and calculating molecular values of XNSB1 and XNSB2 as XNSB1F, XNSB F respectively;
secondly, taking a certain number of XNSB1 and XNSB2 samples, putting the samples into a muffle furnace, burning the samples to constant weight at a certain temperature, taking the samples out, cooling the samples to room temperature, respectively adding sulfuric acid solution for dissolving the samples, adjusting pH to obtain a certain amount of neutral solution, respectively adding a certain amount of ammonia water into the solution to generate blue color, and testing the chromaticity C value of the solution by using a handheld intelligent colorimeter, wherein the chromaticity value is XNSB1CD and XNSB2CD;
and finally, comparing and testing, namely simulating the existence of copper ions in an animal body, preparing a reference quantity containing copper ions with a certain concentration, adding sulfuric acid solution for dissolving, regulating pH value, processing into a certain quantity of neutral solution, respectively generating blue color to a certain quantity of ammonia water in the solution, testing the value of chromaticity CD by using a handheld intelligent colorimeter, comparing and testing to show the quantity and existence state of the copper ions, and judging whether the enzymolysis reaction generates the copper ions in an out-of-standard decomposition state or not according to the molecular weight or the condition of the enzymolysis reaction or the molecular weight according to a corresponding parameter formula by combining the filtration recovery rate of the supernatant fluid of the controlled release substance in the basic performance test with the molecular weight and viscosity of the controlled release substance obtained in the basic performance test.
4. The process for preparing the meat-based enzymatically active pet food having antioxidant activity of claim 2, wherein: the method comprises the following steps of judging and regulating enzymolysis reaction according to test data after the measurement and control release substances participate in the enzymolysis process:
and judging the protein decomposition condition by using the recovery rate of the supernatant fluid filtrate after the measurement and control release substances participate in the enzymolysis process, and then combining the viscosity value after the measurement and control release substances participate in the enzymolysis process, wherein the molecular weight judgment after the measurement and control release substances participate in the enzymolysis process comprises the ionic state condition of copper in the enzymolysis process or the condition of the measurement and control enzymolysis process.
5. The process for preparing the meat-based enzymatically active pet food having antioxidant activity of claim 2, wherein: the method for testing the state of copper ions in enzymolysis by using the controlled release substance comprises the following steps: weighing pretreated meat and animal viscera, performing enzymolysis by using part of processes in the preparation process of the meat enzymolysis pet food with antioxidant activity, wherein the part of processes comprises adjusting the pH value of a solution to 4.5, controlling the temperature to 60 ℃, then hydrolyzing with 3% of pancreatin, chymotrypsin and histidine decarboxylase in equal parts by weight for 1h to form hydrolysate, adding 0.05% of a controlled release substance into supernatant of the hydrolysate to hydrolyze for 0.5h, adjusting the pH value to 8 hydrolysis for 0.5h, taking 100g of supernatant, filtering with filter paper with the aperture of not more than 1 mu m, weighing the filtrate, calculating the recovery value XNSBHS of the supernatant filtrate, judging the chicken protein hydrolysis condition according to the recovery value XNSBHS, drying the filtered filter paper with ethanol to constant weight, marking the filtrate as XNSB, preparing a 0.3 deionized water solution by taking the XNSB, converting the viscosity N into a viscosity value of XNSBN, and calculating the molecular weight according to the following judgment: when the molecular weight of the controlled release substance is less than 200 ten thousand and the filtering recovery rate of the supernatant is more than 93.6%, the controlled release substance is degraded too quickly; when the molecular weight of the controlled release substance is more than 226 ten thousand and the filtering recovery rate of the supernatant is less than 93.6%, the molecular degradation of the controlled release substance is in a basic range.
6. A meat-based enzymatic pet food product made by the process for preparing a meat-based enzymatic pet food product having antioxidant activity as defined in any one of claims 1 to 5, wherein: including the beneficial products which appear after the controlled release substances participate in the enzymolysis process.
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