CN116998612A - Rumen bypass nicotinic acid and preparation method thereof - Google Patents

Rumen bypass nicotinic acid and preparation method thereof Download PDF

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Publication number
CN116998612A
CN116998612A CN202311003194.6A CN202311003194A CN116998612A CN 116998612 A CN116998612 A CN 116998612A CN 202311003194 A CN202311003194 A CN 202311003194A CN 116998612 A CN116998612 A CN 116998612A
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nicotinic acid
rumen
coating
reaction
konjak glucomannan
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李寰旭
张晓明
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Anhui Beijing Oriental Kingherd Biotechnology Co ltd
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Anhui Beijing Oriental Kingherd Biotechnology Co ltd
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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
    • A23K20/163Sugars; Polysaccharides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/20Inorganic substances, e.g. oligoelements
    • A23K20/24Compounds of alkaline earth metals, e.g. magnesium
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K40/00Shaping or working-up of animal feeding-stuffs
    • A23K40/30Shaping or working-up of animal feeding-stuffs by encapsulating; by coating

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Zoology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Animal Husbandry (AREA)
  • Birds (AREA)
  • Inorganic Chemistry (AREA)
  • Fodder In General (AREA)

Abstract

The invention discloses rumen-bypass nicotinic acid and a preparation method thereof, which belong to the technical field of rumen-bypass nicotinic acid.

Description

Rumen bypass nicotinic acid and preparation method thereof
Technical Field
The invention belongs to the technical field of rumen-bypass nicotinic acid, and particularly relates to rumen-bypass nicotinic acid and a preparation method thereof.
Background
The rumen bypass technology, also called rumen protective technology, is to treat nutrient substances by special technology, such as coating, so that the nutrient substances are protected, and the nutrient substances are reduced to be fermented and degraded in the rumen of ruminants and are digested and absorbed after directly entering the small intestine, thereby achieving the purpose of improving the utilization rate of feed. The rumen bypass technology can reduce the degradation rate of nutrients in the rumen of ruminants and increase digestion and absorption in the small intestine, thereby improving the total utilization rate of the nutrients. At present, the rumen bypass nutrient which is researched and applied in the dairy cow production mainly comprises rumen bypass fat, rumen bypass amino acid, rumen bypass choline and the like. The smoke acidity is extremely stable and heat-resistant. The animal must be obtained from the outside. The lack of nicotinic acid, the animals showed slow growth and decreased appetite, and the chickens showed mainly nonspecific symptoms such as stomatitis, poor feather growth, dermatitis, leg bending, swelling, diarrhea, mild anemia and necrotic enteritis. The nicotinic acid also has remarkable pharmacological action, can dilate blood vessels, can make skin red and heat, and can reduce blood fat and cholesterol. The most common methods in coating technology are blood coating and fat coating. Whole blood coating the egg albumin and whey proteins are mixed with the feed and a film is formed on the exterior of the feed pellet. The whole blood coating can be applied to ruminant feed to influence the palatability of ruminants and improve the disease transmission capacity. Fat coating is mainly of two types, fatty acid hydrogenation and fatty acid calcification. Fatty acid hydrogenation is the conversion of unsaturated fatty acids into saturated fatty acids, abbreviated as hydrogenated fats, by chemical hydrogenation. The method mainly uses the principle that the melting point of saturated fatty acid is higher than that of unsaturated fatty acid, so as to improve the melting point of fat, is insoluble in rumen fluid at the temperature of 38-39 ℃ of rumen, has no influence on the activity of rumen microorganisms, and is only dissolved under the action of digestive fluid in small intestine. However, the rumen bypass fatty product has high rumen bypass saturated fatty acid content, so that the digestibility of the rumen bypass fatty product is lower than that of the rumen bypass fatty acid-containing product. Fatty acid calcification is the synthesis of fatty acid calcium salt, short fatty acid calcium, from long chain fatty acid through saponification. Blood products, such as dried plasma, fish meal, bone meal, blood meal, etc., and most animal feeds have been banned from ruminant feeds because of their susceptibility to disease, causing limitations in fat coating, increasing formulation difficulty. The fatty acid calcium is a rumen bypass fatty product which is widely used in biological research and application of dairy cows at present, the product types are great, and the fatty acid calcium can be divided into short chain fatty acid calcium, medium chain fatty acid calcium, long chain fatty acid calcium and the like, and the fatty acid calcium is available in the market and comprises calcium isobutyrate, calcium octoate, calcium caprate, calcium palmitate, calcium stearate and the like, and the fatty acid calcium contains calcium, so that the fat content is limited, the effective energy value is low, the saponification is easy to be insufficient, the quality of the produced product is unstable, the absorption efficiency difference is obvious, and the user is not easy to control; the product contains a certain amount of short chain fatty acid, which affects rumen bypass effect, has soap smell and poor palatability, and cows or milch goats are unwilling to eat. Chinese patent CN110637930A discloses a rumen protected amylase, wherein the main component of the capsule material is saturated fatty acid, acrylic resin IV or chitosan, the acrylic resin IV and the chitosan are not mixed, and the main component of the core material is amylase. The acrylic resin IV can be rapidly dissolved in the pH range below 5, is a tertiary amine cationic compound, forms salt when meeting acid, depends on the effect of the cationic acrylate polymer on the salt formation when meeting acid, is mainly applied to human medicine in the past, has high production cost, unstable product content, poor granularity uniformity and the like, and has low practical value. The rumen bypass is insoluble in the environment with pH value of 5-7, does not interfere the normal activity of rumen microorganism, can smoothly pass through the rumen, but is immediately decomposed in the environment with gastric acidity. One skilled in the art is urgent to develop a rumen bypass nicotinic acid and a preparation method thereof so as to meet the existing application market and performance requirements.
Disclosure of Invention
In view of this, the present invention provides rumen bypass niacin and a method for preparing the same.
The rumen-bypass nicotinic acid comprises a wall material and a core material, wherein the wall material is a double-layer composite material formed by coating oxidized konjak glucomannan with calcium carbonate, the weight ratio of the oxidized konjak glucomannan to the calcium carbonate is 1:1-1.5, the core material is a nicotinic acid pure substance, and the weight ratio of the wall material to the core material is 1:4-4.5.
The preparation method of the rumen bypass nicotinic acid comprises the following steps: firstly, adding isopropanol and konjak glucomannan into a reaction kettle, stirring for 3-5 min, uniformly mixing, regulating the pH value to 7.0-7.5, dropwise adding hydrogen peroxide solution with the mass fraction of 2.5-3% within 20-30 min, continuously reacting for 3-4 h, adding excessive sodium sulfite to terminate the reaction, repeatedly washing the precipitate with 90% alcohol for 3 times, and air-drying at room temperature to obtain oxidized konjak glucomannan; secondly, according to the parts by weight, 65-70 parts of aqueous solution with the mass concentration of 4% -6% is prepared by the oxidized konjak glucomannan in the first step, then 0.002-0.004 part of sodium tripolyphosphate is added, after the reaction is carried out for 2 hours at 45-50 ℃, 0.005-0.01 part of glutaraldehyde aqueous solution with the mass fraction of 2% is added, the temperature is raised to 50-60 ℃ and the temperature is kept for 0.5-1 hour, so as to obtain glue solution, the glue solution is used as coating liquid, nicotinic acid is taken and placed in a fluidized bed coating machine for coating, hot air at 60 ℃ is blown in for drying for 0.5-1 hour, and the obtained konjak glucomannan coated nicotinic acid is obtained; thirdly, taking food-grade lime milk with the mass fraction of 4% -5%, injecting the food-grade lime milk into a reaction kettle, uniformly pouring the konjak glucomannan coated nicotinic acid obtained in the last step into the reaction kettle, starting a carbon dioxide gas cylinder, controlling the flow rate of carbon dioxide, the stirring rotating speed and the reaction temperature, performing reaction coating, performing pH value to be 7.0-7.3 after the reaction coating time is 20-25 min, and performing spray drying to obtain rumen-passing nicotinic acid.
Further, the mass ratio of the konjac glucomannan to the isopropanol in the first step is 1:3-4.
Further, in the third step, the flow rate of carbon dioxide is 15L/h, the stirring speed is 200-250 rpm, and the reaction temperature is 25-30 ℃.
Further, the air outlet temperature of the spray drying in the third step is 85-90 ℃, the atomization frequency is 40Hz, the feeding speed is 12-14 r/min, the relative density of the feed liquid is 1.06-1.08, and the air inlet temperature is 135-145 ℃.
Further, the air inlet temperature of the coating in the second step is 60-65 ℃, the atomization gas pressure is 0.1-0.11 MPa, the peristaltic pump rotating speed is 8-9 r/min, and the fan rotating speed is 1000rpm.
The invention has the beneficial effects that:
according to the invention, oxydol is used for oxidizing konjak glucomannan to prepare oxidized konjak glucomannan for fluidization coating and coating nicotinic acid, and calcium carbonate is continuously coated by adopting a lime milk blowing method, so that a double-layer composite material with a wall material of which the oxidized konjak glucomannan is coated by the calcium carbonate is formed, and the rumen-bypass nicotinic acid with a core material of a nicotinic acid pure substance is obtained. The double-layer composite material coated by calcium carbonate by using the difference of rumen pH value and true stomach pH value is not decomposed in neutral solution but is decomposed in acid environment, so that the double-layer composite material is not degraded in rumen and is digested and utilized after true stomach. The protective film can not be decomposed in the environment with the pH value of 5-7 in rumen, nicotinic acid can not be dissolved out, and in the acidic environment with the pH value of 2-3 in true stomach, the protective film is destroyed, the coated nicotinic acid and the food raw material source are dissolved out, and the protective film has konjak fragrance, is harmless and has no residue and high protection degree.
Compared with the prior art, the invention has the following advantages: the rumen bypass nicotinic acid disclosed by the invention can improve the dry matter feed intake, improve the milk yield, reduce the postpartum body condition loss, promote the body condition recovery, reduce the incidence rate of clinical and subclinical ketosis, reduce the incidence rate of fatty liver syndrome, shorten the postpartum oestrus mating time, relieve the heat stress and greatly reduce the incidence rate of true stomach deflection. Rumen by-pass niacin greatly improves the dry matter feed intake of cows.
Detailed Description
Example 1
KJ-30 superfine konjak glucomannan of the Johnsen konjak company, tripod-marked food-grade hydrogen peroxide, bright-margin food-grade slaked lime, emerging food-grade sodium tripolyphosphate and Zhongrui food-grade nicotinic acid.
The rumen by-pass nicotinic acid comprises a wall material and a core material, and the preparation method comprises the following steps: firstly, adding isopropanol and konjak glucomannan into a reaction kettle, stirring for 5min, uniformly mixing, regulating the pH value to 7.5, dropwise adding hydrogen peroxide solution with the mass fraction of 3% within 30min, keeping the mass of the hydrogen peroxide solution to be 15% of that of the konjak glucomannan, continuously reacting for 4h, adding excessive sodium sulfite to stop the reaction, repeatedly washing and precipitating for 3 times by using 90% alcohol, and airing at room temperature to obtain oxidized konjak glucomannan; secondly, preparing 70 parts of aqueous solution with the mass concentration of 6% by taking the oxidized konjak glucomannan in the first step according to parts by mass, adding 0.004 part of sodium tripolyphosphate, reacting for 2 hours at 50 ℃, adding 0.01 part of glutaraldehyde aqueous solution with the mass fraction of 2%, heating to 60 ℃ and preserving heat for 1 hour to obtain glue solution, taking the glue solution as coating liquid, taking nicotinic acid, placing the nicotinic acid into a fluidized bed coating machine for coating, wherein the air inlet temperature is 65 ℃, the atomizing gas pressure is 0.11MPa, the peristaltic pump rotating speed is 9r/min, the fan rotating speed is 1000rpm, blowing hot air at 60 ℃ for drying for 1 hour, and obtaining the konjak glucomannan coated nicotinic acid; thirdly, taking food-grade lime milk with the mass fraction of 5%, injecting the food-grade lime milk into a reaction kettle, pouring the konjak glucomannan coated nicotinic acid obtained in the last step into the reaction kettle at a constant speed, starting a carbon dioxide gas cylinder, controlling the flow rate of carbon dioxide to be 15L/h, stirring at a speed of 250rpm, performing reaction coating at a reaction temperature of 30 ℃, performing pH value to be 7.3 after the reaction coating time is 25min, performing spray drying, wherein the air outlet temperature of the spray drying is 90 ℃, the atomization frequency is 40Hz, the feeding speed is 14r/min, the relative density of feed liquid is 1.08, and the air inlet temperature is 145 ℃, thus obtaining the rumen-passing nicotinic acid. The wall material is a double-layer composite material with oxidized konjak glucomannan coated by calcium carbonate, wherein the weight ratio of the oxidized konjak glucomannan to the calcium carbonate is 1:1.5, the core material is a nicotinic acid pure substance, and the weight ratio of the wall material to the core material is 1:4.5.
The product is as follows: the color and luster of the particles are uniform and consistent, the moisture content of the particles is 6.0 percent, the analysis sieves with the granularity of 4.0mm pass through the particles completely, and the rumen bypass protection rate is 2h99.89 percent, 4h97.32 percent, 8h92.6 percent and 12h89.7 percent.
The nicotinic acid content of the rumen protected nicotinic acid product is 38.24 percent, and the rumen degradation rate of 8h dry matter measured by a rumen nylon bag method is 15.66 percent; the rumen degradation rate of 8h nicotinic acid is 26.10 percent.
Example 2
Raw materials: consistent konjak company YZ-J-36MY konjak mannan, xinnuhua food-grade hydrogen peroxide, xinyuan food-grade slaked lime, vat Fu food-grade sodium tripolyphosphate and Xingyu chemical food-grade nicotinic acid.
The rumen by-pass nicotinic acid comprises a wall material and a core material, and the preparation method comprises the following steps: firstly, adding isopropanol and konjak glucomannan into a reaction kettle, stirring for 3min, uniformly mixing, regulating the pH value to 7.0, dropwise adding hydrogen peroxide solution with the mass fraction of 2.5% within 20min, wherein the mass fraction of the hydrogen peroxide solution is 10% of that of the konjak glucomannan, continuously reacting for 3h, adding excessive sodium sulfite to terminate the reaction, repeatedly washing the precipitate with 90% alcohol for 3 times, and air-drying at room temperature to obtain oxidized konjak glucomannan; secondly, preparing 65 parts of aqueous solution with the mass concentration of 4% by taking the oxidized konjak glucomannan in the first step according to parts by mass, adding 0.002 part of sodium tripolyphosphate, reacting for 2 hours at 45 ℃, adding 0.005 part of glutaraldehyde aqueous solution with the mass fraction of 2%, heating to 50 ℃ and preserving heat for 0.5 hours to obtain glue solution, taking the glue solution as coating liquid, putting nicotinic acid into a fluidized bed coating machine for coating, wherein the air inlet temperature is 60 ℃, the atomizing gas pressure is 0.1MPa, the peristaltic pump rotating speed is 8r/min, the fan rotating speed is 1000rpm, blowing hot air at 60 ℃ for drying for 0.5 hours, and obtaining the coated nicotinic acid of the oxidized konjak glucomannan; thirdly, taking food-grade lime milk with the mass fraction of 4%, injecting the food-grade lime milk into a reaction kettle, pouring the konjak glucomannan coated nicotinic acid obtained in the last step into the reaction kettle at a constant speed, starting a carbon dioxide gas cylinder, controlling the flow rate of carbon dioxide to be 15L/h, stirring at 200rpm, performing reaction coating at the reaction temperature of 25 ℃, performing pH value to be 7.0 after the reaction coating time is 20min, performing spray drying, wherein the air outlet temperature of the spray drying is 85 ℃, the atomization frequency is 40Hz, the feeding speed is 12r/min, the relative density of feed liquid is 1.06, and the air inlet temperature is 135 ℃, thus obtaining the rumen-passing nicotinic acid. The wall material is a double-layer composite material with oxidized konjak glucomannan coated by calcium carbonate, wherein the weight ratio of the oxidized konjak glucomannan to the calcium carbonate is 1:1, the core material is a nicotinic acid pure substance, and the weight ratio of the wall material to the core material is 1:4.
The product is as follows: the color and luster of the konjak powder are uniform and consistent, the moisture content is less than or equal to 8.0 percent, the analysis sieve with the granularity of 4.0mm passes through the rumen bypass protection rate of 2h99.85 percent, 4h97.32 percent, 8h92.5 percent and 12h89.6 percent. The nicotinic acid content of the rumen protected nicotinic acid product is 38.24 percent, and the rumen degradation rate of 8h dry matter is 15.31 percent by adopting a rumen nylon bag method; the rumen degradation rate of 8h nicotinic acid is 26.15 percent.
Note that: reference is made to the method for testing the stability of niacin and folic acid in the additive premix feed of GB/T7300GB/T17813-2018 (Zhang Like, wang, wang Diming, zhu Haiyan, liu Jianxin, chen Jiang. Research on development and stability of rumen protected niacin [ J ]. Feed industry, 2011 (S2): 64-68). Accurately weighing 5g of coated nicotinic acid, placing in a conical flask with a plug, adding 100ml of water, adding the plug, placing in a water bath shaker at 37 ℃ and 50r/min, taking out at 2, 4, 8 and 12 hours respectively, and filtering to obtain nicotinic acid filter residues. The residue was repeatedly washed with cold distilled water and, after no turbidity, the residual amount of nicotinic acid was measured by GB/T17813-1999. The operation method is briefly described as follows: placing the residue in a 10ml brown volumetric flask, adding 1ml sodium carbonate solution (0.1 mol/l), soaking the sample, adding 7ml extractant, mixing, extracting in ultrasonic water bath for 15min, metering volume to 10ml with extractant, mixing, centrifuging at 3000r/min for 15min, discarding upper layer coagulated oil, and storing in centrifuge tube at 4deg.C under shade. When in measurement, the nicotinic acid concentration is measured by a high performance liquid chromatography method with refrigeration at 4 ℃ through filtering by a 0.45 mu m filter membrane into a small bottle with a cover, and the concentration of the test solution is ensured to be less than or equal to 5 mu g/ml. The protection rate of each rumen-protected niacin was calculated, wherein the test animals were Holstein cattle fitted with permanent rumen fistulas, 18 heads per group. The basic conditions of the test cattle are shown in Table 1. Ration composition (%): baking soda 0.1, mecamylide 1.2, beet pulp particles 0.5, apple pulp particles 0.5, soybean meal 4.3, puffed soybean 1.4, DDGS0.5, whole cotton seed 1.1 corn silage 52.2, alfalfa hay 5.9, cow concentrate 27.5, soybean hull particles 1.9, corn germ meal 0.9, northeast China sheep grass 1.9.

Claims (6)

1. The rumen bypass nicotinic acid is characterized by comprising a wall material and a core material, wherein the wall material is a double-layer composite material formed by coating oxidized konjak glucomannan with calcium carbonate, the weight ratio of the oxidized konjak glucomannan to the calcium carbonate is 1:1-1.5, the core material is a nicotinic acid pure substance, and the weight ratio of the wall material to the core material is 1:4-4.5.
2. The rumen bypass niacin according to claim 1, wherein the preparation method comprises the following steps: firstly, adding isopropanol and konjak glucomannan into a reaction kettle, stirring for 3-5 min, uniformly mixing, regulating the pH value to 7.0-7.5, dropwise adding a hydrogen peroxide solution with the mass fraction of 2.5-3% within 20-30 min, keeping the mass of the hydrogen peroxide solution accounting for 10-15% of the konjak glucomannan, continuously reacting for 3-4 h, adding excessive sodium sulfite to stop the reaction, repeatedly washing and precipitating for 3 times by using 90% alcohol, and airing at room temperature to obtain oxidized konjak glucomannan; secondly, according to the parts by weight, 65-70 parts of aqueous solution with the mass concentration of 4% -6% is prepared by the oxidized konjak glucomannan in the first step, then 0.002-0.004 part of sodium tripolyphosphate is added, after the reaction is carried out for 2 hours at 45-50 ℃, 0.005-0.01 part of glutaraldehyde aqueous solution with the mass fraction of 2% is added, the temperature is raised to 50-60 ℃ and the temperature is kept for 0.5-1 hour, so as to obtain glue solution, the glue solution is used as coating liquid, nicotinic acid is taken and placed in a fluidized bed coating machine for coating, hot air at 60 ℃ is blown in for drying for 0.5-1 hour, and the obtained konjak glucomannan coated nicotinic acid is obtained; thirdly, taking food-grade lime milk with the mass fraction of 4% -5%, injecting the food-grade lime milk into a reaction kettle, uniformly pouring the konjak glucomannan coated nicotinic acid obtained in the last step into the reaction kettle, starting a carbon dioxide gas cylinder, controlling the flow rate of carbon dioxide, the stirring rotating speed and the reaction temperature, performing reaction coating, performing pH value to be 7.0-7.3 after the reaction coating time is 20-25 min, and performing spray drying to obtain rumen-passing nicotinic acid.
3. The rumen bypass nicotinic acid according to claim 2, wherein the mass ratio of konjac glucomannan to isopropyl alcohol in the first step is 1:3-4.
4. The rumen bypass nicotinic acid according to claim 2, wherein the flow rate of carbon dioxide in the third step is 15L/h, the stirring speed is 200-250 rpm, and the reaction temperature is 25-30 ℃.
5. The rumen by-pass nicotinic acid according to claim 2, wherein the spray drying air outlet temperature in the third step is 85-90 ℃, the atomization frequency is 40Hz, the feeding speed is 12-14 r/min, the relative density of feed liquid is 1.06-1.08, and the air inlet temperature is 135-145 ℃.
6. The rumen bypass nicotinic acid according to claim 2, wherein the air inlet temperature of the coating in the second step is 60-65 ℃, the atomization gas pressure is 0.1-0.11 MPa, the peristaltic pump rotating speed is 8-9 r/min, and the fan rotating speed is 1000rpm.
CN202311003194.6A 2023-08-10 2023-08-10 Rumen bypass nicotinic acid and preparation method thereof Pending CN116998612A (en)

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CN116998612A true CN116998612A (en) 2023-11-07

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