CN112006172A - Novel rumen-bypass pantothenic acid coating process - Google Patents

Novel rumen-bypass pantothenic acid coating process Download PDF

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Publication number
CN112006172A
CN112006172A CN202010912741.2A CN202010912741A CN112006172A CN 112006172 A CN112006172 A CN 112006172A CN 202010912741 A CN202010912741 A CN 202010912741A CN 112006172 A CN112006172 A CN 112006172A
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solution
pantothenic acid
stirring
coating process
rumen
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Chinese (zh)
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李寰旭
赵鑫源
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Beijing Dongfang Tianhe Rumen Technology Research Institute Co ltd
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Beijing Dongfang Tianhe Rumen Technology Research Institute Co ltd
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Priority to CN202010912741.2A priority Critical patent/CN112006172A/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K50/00Feeding-stuffs specially adapted for particular animals
    • A23K50/10Feeding-stuffs specially adapted for particular animals for ruminants
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/10Organic substances
    • A23K20/174Vitamins
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K40/00Shaping or working-up of animal feeding-stuffs

Abstract

The invention relates to the technical field of rumen bypass vitamins, in particular to a novel rumen bypass pantothenic acid coating process which comprises the steps of preparing a core material solution, preparing a sodium carboxymethyl cellulose solution, preparing a gelatin solution, preparing a paraffin mixed solution, adding the sodium carboxymethyl cellulose solution and the gelatin solution into the paraffin mixed solution for emulsification, dissolving ethyl cellulose and polyethylene, mixing the solutions for high-speed dispersion, cooling for crystallization, washing and filtering crystallized particles, freeze-drying and the like; the invention prepares common pantothenic acid into novel rumen-protected pantothenic acid by a special treatment means, which has the advantages of rumen degradation resistance, high biological activity, high bioavailability, easy absorption, reduced dosage of feed pantothenic acid and lowered culture cost for farmers.

Description

Novel rumen-bypass pantothenic acid coating process
Technical Field
The invention relates to the technical field of rumen-bypass vitamins, in particular to a novel rumen-bypass pantothenic acid coating process.
Background
The energy is used as a limiting factor for the growth and development of the ruminant, and the normal growth and metabolism of the ruminant can be ensured only by meeting the protein requirement on the premise of meeting the energy. Energy in feed provides nutrients, mainly carbohydrates and fats, necessary for the survival of the animals. In recent years, due to the shortage of feed resources, the feed becomes a restriction factor for the development of animal husbandry.
Pantothenic acid can promote fatty acid metabolism, and D-type pantothenic acid starts from the catalytic action of phosphokinase, is converted into COA under the action of a series of enzymes, participates in the metabolism of carbohydrates in vivo, particularly tricarboxylic acid circulation, and simultaneously releases energy for the body to utilize. Researches show that the pantothenic acid is supplemented into low-energy daily ration of the ruminant to promote the energy metabolism, make up the deficiency of the energy in the feed, promote the rumen fermentation and maintain the normal physiological function, promote the growth and development of the animal and reduce the breeding cost. However, due to the action of rumen microorganisms, if pantothenic acid is fed without treatment by direct addition to the basal diet, the vast majority of the pantothenic acid is degraded in the rumen and can reach the small intestine for a very small amount of use. Therefore, aiming at the defects of low rumen degradation resistance, low bioavailability and the like when the existing pantothenic acid is directly added into basic daily ration for feeding, the novel rumen-bypass pantothenic acid coating process which has the advantages of rumen degradation resistance, high bioactivity, high bioavailability, easy absorption and capability of reducing the using amount of feed pantothenic acid is designed to solve the technical problem.
Disclosure of Invention
The invention aims to provide a novel rumen-protected pantothenic acid preparation method, which has important theoretical and practical values for relieving degradation of pantothenic acid in rumen and effectively improving the utilization effect of the pantothenic acid.
The invention is realized by the following technical scheme:
a novel rumen-protected pantothenic acid coating process comprises the following preparation steps:
1) placing a proper amount of pantothenic acid into a reagent bottle containing purified water, then placing into a constant-temperature water bath shaking table, heating and dissolving to obtain a solution A after fully mixing and dissolving;
2) weighing 1 part by weight of sodium carboxymethylcellulose, adding the sodium carboxymethylcellulose into 80-120 parts by weight of deionized water, heating and stirring until the sodium carboxymethylcellulose is completely dissolved to obtain a solution B, pouring the solution B into a high-pressure homogenizer, carrying out high-pressure homogenization under 40-60 MPa, and repeating the high-pressure homogenization for 2-4 times;
3) weighing 1 part by weight of gelatin, adding the gelatin into 80-120 parts by weight of deionized water, heating and stirring until the gelatin is completely dissolved to obtain a solution C, pouring the solution C into a high-pressure homogenizer, homogenizing under high pressure of 40-60 MPa, and repeating the high-pressure homogenization for 2-4 times;
4) taking 1000 parts of liquid paraffin and 1-3 parts of sorbitan monooleate according to the volume ratio, and uniformly mixing the liquid paraffin and the sorbitan monooleate to obtain a solution D;
5) mixing and stirring the solution B prepared in the step 2 and the solution C prepared in the step 3 according to the volume of 1:1 for 10-15 min, then adding the stirred solution into the solution D, wherein the volume ratio of the solution D to the solution B to the solution C is 1:2:2, carrying out ultrasonic emulsification for 5-10 min, immediately transferring into a low-temperature water bath kettle, and stirring for 30-60 min at the temperature of 20-25 ℃ to obtain a solution E;
6) adding ethyl cellulose and polyethanol into an organic solvent according to the mass ratio of 1:1, heating and stirring until the ethyl cellulose and the polyethanol are completely dissolved, homogenizing under high pressure of 40-60 MPa, and repeating the high-pressure homogenization for 2-4 times to obtain a solution F;
7) mixing the solution A prepared in the step 1 and the solution E prepared in the step 5 in a ratio of (10-12): 5, dispersing the mixture in a high-speed refiner at a rotating speed of 6000 to 10000r/min for 30 to 50s, repeating the high-speed dispersion treatment for 2 to 4 times, and then using an electric stirrer at a temperature of between 70 and 80 ℃ for 20 to 25 min;
8) adding the solution F prepared in the step 6 into the mixed solution stirred in the step 7, wherein the volume ratio of the solution F to the mixed solution stirred in the step 7 is 2: (7-9), continuously stirring for 20-30 min, then slowly reducing the temperature to reduce the solubility of the ethyl cellulose for cooling and solidification to obtain granular crystals, washing and filtering with an organic solvent, and freeze-drying in a vacuum freeze-drying machine after washing and filtering to obtain rumen-bypass pantothenic acid.
Preferably, the weight ratio of pantothenic acid to purified water in the step 1 is 1: 1.
preferably, the heating dissolution temperature in the step 1 is 80 ℃, and the operation is carried out for 30 min.
Preferably, the heating and stirring temperature in the step 2 is 80 ℃, and the stirring speed is 200-400 r/min.
Preferably, the heating and stirring temperature in the step 3 is 50 ℃, and the stirring speed is 200-400 r/min.
Preferably, the heating and stirring temperature in the step 6 is 80 ℃, and the stirring speed is 400-600 r/min.
Preferably, the organic solvent in step 6 and step 8 is cyclohexane.
Preferably, the diameter of the granular crystal in the step 8 is 0.8-1 mm.
Has the advantages that:
the novel rumen-bypass pantothenic acid coating process disclosed by the invention has the advantages that after pantothenic acid is coated and treated, the rumen-bypass rate of the novel rumen-bypass pantothenic acid obtained by the novel rumen-bypass pantothenic acid in 12 hours is up to more than 80%, and the novel rumen-bypass pantothenic acid is added into basic ration for feeding, wherein most rumen-bypass pantothenic acid can be absorbed and utilized by the small intestine of ruminants, so that the energy metabolism of the ruminants can be promoted, the deficiency of energy in feed is compensated, rumen fermentation is promoted, normal physiological functions are maintained, and the growth; the rumen-bypass pantothenic acid prepared by the coating process has the beneficial effects of rumen degradation resistance, high biological activity, high bioavailability, easy absorption and capability of reducing the dosage of feed pantothenic acid, effectively reduces the culture cost of farmers, and has obvious effect.
Detailed Description
Example 1
A novel rumen bypass pantothenic acid coating process comprises the following eight preparation steps:
1) preparing a core material solution:
mixing pantothenic acid and purified water in a ratio of 1:1, placing the pantothenic acid and the purified water into a reagent bottle containing the purified water, placing the reagent bottle into a constant-temperature water bath shaking table, heating to 80 ℃, and running for 30min to fully mix and dissolve the pantothenic acid and the purified water to obtain a solution A.
2) Preparing a sodium carboxymethyl cellulose solution:
accurately weighing 1 part by weight of CMC (sodium carboxymethylcellulose), slowly adding into 99 parts by weight of deionized water, stirring at a stirring speed of 350r/min and at a temperature of 80 ℃ by using an electric stirrer until the CMC is completely dissolved to obtain a solution B, pouring the solution B into a high-pressure homogenizer, homogenizing under a high pressure of 50MPa, and repeating the high-pressure homogenization treatment for 3 times by using the same parameters.
3) Preparing a gelatin solution:
accurately weighing 1 part by weight of gelatin, slowly adding the gelatin into 99 parts by weight of deionized water, stirring the gelatin at a stirring speed of 350r/min and a temperature of 50 ℃ by using an electric stirrer until the gelatin is completely dissolved to obtain a solution C, homogenizing the solution C under high pressure of 50MPa, and repeating the high-pressure homogenization treatment for 3 times by using the same parameters.
4) Preparing a paraffin mixed solution:
selecting liquid paraffin according to paraffin HLB, taking 1000 parts of liquid paraffin and 1 part of sorbitan monooleate (sPan-80) according to volume ratio, and uniformly mixing the liquid paraffin and the sorbitan monooleate to obtain solution D.
5) Mixing the solution B prepared in the step 2 and the solution C prepared in the step 3 according to the volume of 1:1, stirring for 10min, then adding the stirred solution into the solution D, wherein the volume ratio of the solution D to the solution B to the solution C is 1:2:2, immediately carrying out ultrasonic emulsification for 8min, then transferring into a low-temperature water bath kettle, and stirring for 40min at the temperature of 20 ℃ to obtain a solution E.
6) Adding ethyl cellulose and polyethanol into cyclohexane organic solvent according to the mass ratio of 1:1, heating to 80 ℃, stirring at the rotating speed of 500r/min until the ethyl cellulose and the polyethanol are completely dissolved, then homogenizing under high pressure of 50MPa, and repeating the high-pressure homogenization treatment for 3 times according to the same parameters to obtain a solution F.
7) Mixing the solution A prepared in the step 1 and the solution E prepared in the step 5 in a ratio of 11: 5, dispersing in a high-speed homogenizer at a rotation speed of 10000r/min for about 30s, repeating the high-speed dispersion treatment 3 times, and then stirring with an electric stirrer at 80 ℃ for 20 min.
8) Adding the solution F prepared in the step 6 into the mixed solution stirred in the step 7, wherein the volume ratio of the solution F to the mixed solution stirred in the step 7 is 1: and 4, continuously stirring for 25min, slowly reducing the temperature to reduce the solubility of the ethyl cellulose so as to cool and solidify to obtain granular crystals with the diameter of 0.8-1 mm, washing and filtering by using a cyclohexane organic solvent, and freeze-drying in a vacuum freeze dryer after washing and filtering to obtain rumen-bypass pantothenic acid.
Example 2
A novel rumen bypass pantothenic acid coating process comprises the following eight preparation steps:
1) preparing a core material solution:
mixing pantothenic acid and purified water in a ratio of 1:1, placing the pantothenic acid and the purified water into a reagent bottle containing the purified water, placing the reagent bottle into a constant-temperature water bath shaking table, heating to 80 ℃, and running for 30min to fully mix and dissolve the pantothenic acid and the purified water to obtain a solution A.
2) Preparing a sodium carboxymethyl cellulose solution:
accurately weighing 1 part by weight of CMC (sodium carboxymethylcellulose), slowly adding into 110 parts by weight of deionized water, stirring at a stirring speed of 300r/min and a temperature of 80 ℃ by using an electric stirrer until the CMC is completely dissolved to obtain a solution B, pouring the solution B into a high-pressure homogenizer, homogenizing under a high pressure of 45MPa, and repeating the high-pressure homogenization treatment for 3 times by using the same parameters.
3) Preparing a gelatin solution:
accurately weighing 1 part by weight of gelatin, slowly adding the gelatin into 110 parts by weight of deionized water, stirring the gelatin at a stirring speed of 300r/min and a temperature of 50 ℃ by using an electric stirrer until the gelatin is completely dissolved to obtain a solution C, homogenizing the solution C under high pressure of 45MPa, and repeating the high-pressure homogenization treatment for 3 times according to the same parameters.
4) Preparing a paraffin mixed solution:
selecting liquid paraffin according to paraffin HLB, taking 1000 parts of liquid paraffin and 2 parts of sorbitan monooleate (sPan-80) according to volume ratio, and uniformly mixing the liquid paraffin and the sorbitan monooleate to obtain solution D.
5) Mixing and stirring the solution B prepared in the step 2 and the solution C prepared in the step 3 according to the volume of 1:1 for 15min, then adding the stirred solution into the solution D, wherein the volume ratio of the solution D to the solution B to the solution C is 1:2:2, immediately carrying out ultrasonic emulsification for 10min, and then immediately transferring the solution into a low-temperature water bath kettle to stir for 30min at the temperature of 25 ℃ to obtain a solution E.
6) Adding ethyl cellulose and polyethanol into cyclohexane organic solvent according to the mass ratio of 1:1, heating to 80 ℃, stirring at the rotating speed of 500r/min until the ethyl cellulose and the polyethanol are completely dissolved, then homogenizing under high pressure of 45MPa, and repeating the high-pressure homogenization treatment for 3 times according to the same parameters to obtain a solution F.
7) Mixing the solution A prepared in the step 1 and the solution E prepared in the step 5 in a ratio of 12: 5, dispersing the mixture in a high-speed homogenizer at a rotation speed of 80000r/min for about 45 seconds, repeating the high-speed dispersion treatment 3 times, and then stirring the mixture at 80 ℃ for 20 minutes with an electric stirrer.
8) Adding the solution F prepared in the step 6 into the mixed solution stirred in the step 7, wherein the volume ratio of the solution F to the mixed solution stirred in the step 7 is 2: and 7, continuously stirring for 28min, slowly reducing the temperature to reduce the solubility of the ethyl cellulose so as to cool and solidify to obtain granular crystals with the diameter of 0.8-1 mm, washing and filtering by using a cyclohexane organic solvent, and freeze-drying in a vacuum freeze dryer after washing and filtering to obtain rumen-bypass pantothenic acid.
Evaluation of rumen bypass rate performance of the novel rumen bypass pantothenic acid prepared in example 1 and example 2:
the rumen degradation rates of the novel rumen-protected pantothenic acid obtained by coating treatment in the above examples 1 and 2 and the pantothenic acid without coating treatment at 4 culture points at 2, 6, 12 and 24 hours were respectively measured by a rumen nylon bag method using 4 holstein lactating cows with permanent rumen fistulas as test animals. The results of the measurements on 1 plastic tube (2 nylon bags) per cow per time point are shown in table 1 below. The data in table 1 below are the average of 8 replicates.
Specifically, the rumen degradation rate is calculated as follows:
rumen degradation rate = (degradation amount of rumen-bypass pantothenic acid ¸ corrected for the weight of packaged rumen-bypass pantothenic acid at a certain culture time point)' 100%;
the amount of rumen bypass pantothenic acid degraded at a time point = corrected amount of rumen bypass pantothenic acid bagged-amount of rumen bypass pantothenic acid at a culture time point;
corrected packaged rumen bypass pantothenate weight = actual packaged rumen bypass pantothenate weight ″ (1-rumen bypass pantothenate packaged escape rate);
rumen bypass pantothenic acid bagging escape rate (%) = [ (weight of rumen bypass pantothenic acid in blank-weight of rumen bypass pantothenic acid residue in blank) ¸ is 100% of the weight of rumen bypass pantothenic acid in blank;
the results are shown in Table 1
Table 1: degradation ratio (%)% of rumen-protected pantothenic acid measured by nylon bag method
2(h) 6(h) 12(h) 24(h)
Example 1 8.19 10.02 17.28 24.38
Example 2 8.24 10.28 17.13 24.21
Uncoated pantothenic acid 92.02 94.17 96.39 98.05
The determination result shows that the non-coated pantothenic acid is basically degraded at 12 h; the rumen-protected pantothenic acid coated by the process in the examples 1 and 2 is cultured in rumen for 12 hours, the degradation rate is about 17%, and the rumen-protected pantothenic acid developed by the process has a 12-hour rumen-protected rate of over 80% and a remarkable effect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (8)

1. A novel rumen-protected pantothenic acid coating process is characterized by comprising the following preparation steps:
1) placing a proper amount of pantothenic acid into a reagent bottle containing purified water, then placing into a constant-temperature water bath shaking table, heating and dissolving to obtain a solution A after fully mixing and dissolving;
2) weighing 1 part by weight of sodium carboxymethylcellulose, adding the sodium carboxymethylcellulose into 80-120 parts by weight of deionized water, heating and stirring until the sodium carboxymethylcellulose is completely dissolved to obtain a solution B, pouring the solution B into a high-pressure homogenizer, carrying out high-pressure homogenization under 40-60 MPa, and repeating the high-pressure homogenization for 2-4 times;
3) weighing 1 part by weight of gelatin, adding the gelatin into 80-120 parts by weight of deionized water, heating and stirring until the gelatin is completely dissolved to obtain a solution C, pouring the solution C into a high-pressure homogenizer, homogenizing under high pressure of 40-60 MPa, and repeating the high-pressure homogenization for 2-4 times;
4) taking 1000 parts of liquid paraffin and 1-3 parts of sorbitan monooleate according to the volume ratio, and uniformly mixing the liquid paraffin and the sorbitan monooleate to obtain a solution D;
5) mixing and stirring the solution B prepared in the step 2 and the solution C prepared in the step 3 according to the volume of 1:1 for 10-15 min, then adding the stirred solution into the solution D, wherein the volume ratio of the solution D to the solution B to the solution C is 1:2:2, carrying out ultrasonic emulsification for 5-10 min, immediately transferring into a low-temperature water bath kettle, and stirring for 30-60 min at the temperature of 20-25 ℃ to obtain a solution E;
6) adding ethyl cellulose and polyethanol into an organic solvent according to the mass ratio of 1:1, heating and stirring until the ethyl cellulose and the polyethanol are completely dissolved, homogenizing under high pressure of 40-60 MPa, and repeating the high-pressure homogenization for 2-4 times to obtain a solution F;
7) mixing the solution A prepared in the step 1 and the solution E prepared in the step 5 in a ratio of (10-12): 5, dispersing the mixture in a high-speed refiner at a rotating speed of 6000 to 10000r/min for 30 to 50s, repeating the high-speed dispersion treatment for 2 to 4 times, and then using an electric stirrer at a temperature of between 70 and 80 ℃ for 20 to 25 min;
8) adding the solution F prepared in the step 6 into the mixed solution stirred in the step 7, wherein the volume ratio of the solution F to the mixed solution stirred in the step 7 is 2: (7-9), continuously stirring for 20-30 min, then slowly reducing the temperature to reduce the solubility of the ethyl cellulose for cooling and solidification to obtain granular crystals, washing and filtering with an organic solvent, and freeze-drying in a vacuum freeze-drying machine after washing and filtering to obtain rumen-bypass pantothenic acid.
2. The novel rumen bypass pantothenic acid coating process according to claim 1, wherein: in the step 1, the weight ratio of pantothenic acid to purified water is 1: 1.
3. the novel rumen bypass pantothenic acid coating process according to claim 1, wherein: the heating and dissolving temperature in the step 1 is 80 ℃, and the operation is carried out for 30 min.
4. The novel rumen bypass pantothenic acid coating process according to claim 1, wherein: the heating and stirring temperature in the step 2 is 80 ℃, and the stirring speed is 200-400 r/min.
5. The novel rumen bypass pantothenic acid coating process according to claim 1, wherein: the heating and stirring temperature in the step 3 is 50 ℃, and the stirring speed is 200-400 r/min.
6. The novel rumen bypass pantothenic acid coating process according to claim 1, wherein: the heating and stirring temperature in the step 6 is 80 ℃, and the stirring speed is 400-600 r/min.
7. The novel rumen bypass pantothenic acid coating process according to claim 1, wherein: the organic solvent in the step 6 and the organic solvent in the step 8 are both cyclohexane.
8. The novel rumen bypass pantothenic acid coating process according to claim 1, wherein: the diameter of the granular crystal in the step 8 is 0.8-1 mm.
CN202010912741.2A 2020-09-03 2020-09-03 Novel rumen-bypass pantothenic acid coating process Pending CN112006172A (en)

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Publication number Priority date Publication date Assignee Title
CN112868912A (en) * 2021-02-02 2021-06-01 北京东方天合过瘤胃技术研究院有限公司 Preparation method of novel rumen-bypass glucose oxidase

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Application publication date: 20201201