Rumen by-pass preparations, methods for their production and use

Abstract

The application relates to a kind of over rumen preparation and its preparation method and application.The preparation method of the over rumen preparation includes the following steps: taking nutrient and oil, emulsifier, water emulsification, preparation oil-in-water emulsion system;With the oil-in-water emulsion system, core is prepared by granulation;Another nutrient and oil, emulsifier, water emulsification, preparation water-in-oil emulsion system;The water-in-oil emulsion system is covered on the surface of the core, and the first layer coating is prepared;Another oil is melted, and the melted oil is covered on the surface of the first layer coating, and the second layer coating is prepared.The over rumen preparation can effectively pass through the rumen, and can be fully released in small intestine and absorbed by animals.

Description

Technical Field

[0001] This application relates to the field of animal diet technology, and in particular to a rumen-exposed preparation, its preparation method, and its application. Background Technology

[0002] In recent years, the dairy farming industry has developed rapidly, with large-scale farms gradually replacing small farms and cooperative farming models. Many problems in dairy farming are significant factors affecting farm profitability. For example, after calving, dairy cows experience changes in physiology, feed, environment, and management, leading to increased energy needs for maintenance and production. Dry matter intake is low, requiring the cows to utilize large amounts of body fat to provide energy and raw materials for metabolic reactions and milk fat synthesis, resulting in a negative energy balance and potentially causing ketosis, subclinical ketosis, or fatty liver disease. Successfully navigating the peripartum period is a major challenge for dairy producers and farms. The success of this transition determines the cow's production performance, and reducing liver fat accumulation and accelerating its removal from the liver are crucial for a successful transition. Appropriate supplementation with glucose, choline, or niacin is a nutritional solution for controlling ketosis in dairy cows.

[0003] Glucose is an essential nutrient for animal life and production activities. It directly participates in metabolic processes as an energy and carbon source. Appropriate supplementation with exogenous glucose in early lactation increases the amount of glucose that can be absorbed in the small intestine, raising blood glucose levels. This is an effective strategy for preventing and treating postpartum glucose metabolism imbalance in dairy cows, reducing disease incidence, and increasing milk production. Choline is an important component of very low-density lipoprotein (VLDL) and also a methyl donor for carnitine during fatty acid oxidation. Adding choline can promote fatty acid oxidation in the liver while accelerating its transport out of the liver, preventing its deposition. Adding choline can conserve methionine (the most important limiting amino acid in lactating cows) used to provide methyl groups, allowing more methionine to be used for milk production. Niacin, also known as nicotinic acid, is a water-soluble B vitamin. After entering the animal body, it is converted into bioactive nicotinamide (NAM). As a component of nicotinamide adenine dinucleotide (NAD) and nicotinamide adenine dinucleotide phosphate (NADP), these components promote the oxidation of fatty acids and ketone bodies for energy supply during oxidative respiration, reducing ketone body accumulation. Simultaneously, they promote gluconeogenesis, improve glucose supply, and alleviate postpartum energy imbalance. Numerous studies both domestically and internationally have shown that methionine and lysine are the first or second limiting amino acids in the synthesis of milk protein in lactating cows. Rumen-protected amino acids can provide dairy cows with metabolizable amino acids in the small intestine. By adjusting the proportion of metabolizable amino acids in the small intestine through different addition amounts, the amino acid balance can be improved, thereby increasing feed protein utilization, promoting the utilization of free amino acids by mammary tissue, reducing urea nitrogen content in milk and blood, increasing milk protein content and milk yield, reducing dietary protein levels and feed costs, and improving the reproductive performance of cows.

[0004] However, due to the unique digestive physiology of dairy cows, nutrients such as glucose, choline, niacin, methionine, and lysine, when directly fed, will be degraded and utilized by microorganisms in the rumen and cannot be effectively absorbed in the small intestine. Therefore, physical or chemical methods (i.e., rumen protection technology) are needed to protect these nutrients from being broken down by rumen microorganisms, allowing them to safely pass through the rumen and reach the abomasum and small intestine for release.

[0005] Traditional technologies for producing rumen-protected products mainly fall into two categories:

[0006] The first type involves mixing nutrients into a molten coating material to form a mixture. This mixture is then sprayed under sufficient air pressure through a nozzle with multiple small holes. The mixture is sprayed from a temperature environment above its melting point into an airflow below its melting point, where it solidifies to form microspheres containing both a core and a coating material. For example, one method involves adding glucose and a pH-sensitive agent to molten saturated fatty acids and stirring until homogeneous. The mixture is then sprayed through a high-pressure nozzle into a fluidized bed circulated with cold air to obtain rumen-protected glucose particles. Alternatively, another method involves dispersing glucose and a pH-sensitive agent in molten solid vegetable oil, atomizing and solidifying the mixture using a centrifugal atomizer to obtain spherical particles, which are then mixed with an anti-caking agent to obtain a rumen-protected nutrient preparation product.

[0007] The main problem with the first type of method is that water-soluble nutrients are immiscible with oils, resulting in uneven nutrient content in the product. In addition, in order for the oils to disperse the nutrients and exert a certain protective effect, the nutrient content in the product is usually low. Furthermore, the rumen-passing effect is also poor.

[0008] The second type involves mixing nutrient powder, binder, and other excipients, adding a small amount of water to create a wet material, and then granulating, shot-blasting, drying, and sieving to form uniform granules containing nutrients. The outer coating is achieved using traditional fluidized bed technology, allowing the granules to flow freely between each other. This atomizes the coating material into fine droplets, which contact and cover the surface as the granules move. The molten coating material crystallizes at a temperature below its melting point, forming microcapsules. For example, one method involves adding water to glucose and thermostable lipase in a specific ratio to create a wet material, extruding it using an extruder, shot-blasting it, and drying it to obtain glucose microspheres. These microspheres are then fluidized in a fluidized bed, and finally, molten fatty alcohols or saturated fatty acids containing pH-sensitive substances are sprayed onto the surface of the microspheres to obtain rumen-protected glucose granules. Alternatively, another method involves mixing glucose and excipients evenly, adjusting with water, granulating, shot-blasting, drying, and sieving to obtain granules. Molten rumen-protected fat powder is then sprayed onto the surface of the granules using a fluidized bed granulation and coating machine bottom spraying process to obtain rumen-protected glucose.

[0009] The main problem with the second type of method is that it is not suitable for granulating certain nutrients. For example, glucose. During the extrusion granulation process, the glucose generates heat through friction with the extruder and screw. When heated, the glucose softens and becomes sticky, causing it to stick to the cutting blade during cutting and resulting in uneven granule cuts, making it unsuitable for continuous production. In addition, the passage of food through the rumen is a continuous and dynamic process. This type of method can easily lead to over-coating of nutrients that pass through the rumen first. Nutrients with high rumen passage rates are not released in the small intestine, while nutrients that pass through the rumen later are degraded by rumen microorganisms due to prolonged rumen retention, resulting in low overall bioavailability. Summary of the Invention

[0010] Based on this, this application provides a rumen-passing preparation that can effectively pass through the rumen and be fully released in the small intestine for absorption and utilization by animals, as well as its preparation method and application.

[0011] The first aspect of this application provides a method for preparing a rumen-protected preparation, comprising the following steps:

[0012] Nutrients are emulsified with oils, emulsifiers, and water to prepare an oil-in-water emulsion system.

[0013] The core is prepared by granulation using the oil-in-water emulsion system described above;

[0014] Nutrients were emulsified with oils, emulsifiers, and water to prepare a water-in-oil emulsion system.

[0015] The water-in-oil emulsion system is coated onto the surface of the core to prepare a first coating layer.

[0016] Take another oil and melt it. Apply the melted oil to the surface of the first coating layer to prepare the second coating layer.

[0017] In some embodiments, the nutrient is one or more of glucose, choline, lysine, methionine, and niacin.

[0018] In some embodiments, the core preparation step has at least one of the following features:

[0019] (1) The mass ratio of the emulsifier, the oil and the nutrient is (1-10):(3-38):100, and can be (1-4):(7-18):100;

[0020] (2) The mass ratio of water to nutrients is (25-100):100;

[0021] (3) The emulsifier is one or more of polyoxyethylene (8) stearate, polyoxyethylene (20) glyceryl stearate, polyoxyethylene sorbitan esters and fatty acid salts;

[0022] (4) The oil is a fatty acid having 14 or more carbon atoms; further optionally, the oil is one or more of stearic acid, soybean oil, rapeseed oil, sunflower oil, cottonseed oil, rice bran oil, corn oil, peanut oil, coconut oil, hydrogenated palm oil, rice bran wax, beeswax and carnauba wax.

[0023] In some embodiments, the preparation of the core includes the following steps:

[0024] The water and the nutrients are mixed at a temperature of 60℃~80℃ to prepare an aqueous phase;

[0025] The emulsifier is mixed with the molten oil to prepare an oil phase;

[0026] The oil phase is added to the aqueous phase and emulsified to prepare the oil-in-water emulsion system.

[0027] In some embodiments, the preparation of the aqueous phase also includes the step of adding a thickener;

[0028] Optionally, the thickener includes one or more of xanthan gum, gum arabic, pectin, acid-modified starch, sodium carboxymethyl cellulose, and hydroxypropyl methyl cellulose;

[0029] Optionally, the mass ratio of the thickener to the nutrient is (0.5-7):100, or optionally (1-4):100.

[0030] In some embodiments, the granulation method is spray granulation;

[0031] Optionally, the conditions for spray granulation include: granulation temperature of 10℃~25℃, feed flow rate of 600kg / h~1200kg / h, and inlet air humidity of 0%~5%.

[0032] In some embodiments, a drying step is also included after granulation;

[0033] Optionally, the drying conditions include a temperature of 40℃ to 50℃ and a time of 30 min to 60 min.

[0034] In some embodiments, the step of preparing the first coating layer has at least one of the following features:

[0035] (1) The mass ratio of the oil, the emulsifier and the nutrient is (100-233):(1.5-12):100, and can be (115-223):(3-10):100;

[0036] (2) The mass ratio of water to nutrients can be selected as (25-100):100;

[0037] (3) The emulsifier is one or more of the following: monoglycerides and diglycerides, glyceryl monostearate, glyceryl acetate, glyceryl lactate, propylene glycol esters, stearoyl lactate, and sorbitan esters;

[0038] (4) The oil is a fatty acid having 14 or more carbon atoms; further optionally, the oil is one or more of stearic acid, tristearate, coconut oil, hydrogenated palm oil, beeswax and carnauba wax.

[0039] In some embodiments, preparing the first coating layer includes the following steps:

[0040] The water and the nutrients are mixed at 60°C to 80°C to prepare an aqueous phase;

[0041] The emulsifier is mixed with the molten oil to prepare an oil phase;

[0042] The aqueous phase is added to the oil phase and emulsified to prepare the water-in-oil emulsion system;

[0043] The water-in-oil emulsion system is coated onto the surface of the core at a temperature of 30℃ to 60℃, and then cooled to prepare the first coating layer.

[0044] In some embodiments, in the step of preparing the second coating, the oil is a fatty acid having 14 or more carbon atoms; further optionally, the oil is one or more of stearic acid, tristearate, coconut oil, hydrogenated palm oil, beeswax, and carnauba wax.

[0045] In some embodiments, preparing the second coating layer includes the following steps:

[0046] The molten grease is coated onto the surface of the first coating layer at a temperature of 40℃ to 80℃.

[0047] A second aspect of this application provides a rumen-protected preparation obtained by the preparation method described in the first aspect.

[0048] In some embodiments, the rumen-protected formulation has at least one of the following features:

[0049] (1) The total weight of the nutrients accounts for 40% to 70% of the total weight of the rumen-protected preparation, and may be 45% to 67%;

[0050] (2) The particle size of the rumen-exposed preparation is 0.8 mm to 1.4 mm;

[0051] (3) The moisture content of the rumen-protected preparation is 0-3%.

[0052] A third aspect of this application provides the use of the rumen-protected preparation described in the second aspect in the preparation of animal diets.

[0053] The above-described method for preparing rumen-protected formulations involves using an oil-in-water emulsion system to prepare the core, ensuring uniform dispersion of water-soluble nutrients and effectively increasing the overall nutrient content of the formulation. Then, an oil-in-water emulsion system is used to coat the core surface with a first coating layer. This increases the rumen passage rate by reducing the specific surface area of ​​the core and increasing the oil content, while simultaneously reducing the amount of outer oil coating and improving the small intestinal release rate. Finally, a second coating layer is formed by directly coating the first coating layer with oil, effectively separating the nutrients from the rumen fluid and further improving the rumen passage rate. In summary, the resulting rumen-protected formulation has a high nutrient content, with minimal oil degradation in the rumen, while being easily degraded by lipases in the small intestine. As the formulation passes through the rumen → abomasum → small intestine, the two coating layers in the rumen provide good protection for the active substances, improving the rumen passage rate. Upon reaching the small intestine, the oil in the coating is fully decomposed, increasing the small intestinal release rate of nutrients and thus enhancing bioavailability.

[0054] In addition, the above-mentioned method for preparing rumen-protected preparations has the following advantages:

[0055] (1) The prepared rumen-protected preparation has uniform particles, good flowability, and good physical morphology. It is easy to use directly in production, effectively reducing the incidence of peripartum ketosis and fatty liver in dairy cows, improving the health of animals, and increasing the milk yield and milk quality of dairy cows.

[0056] (2) The two-layer coating can effectively reduce mechanical wear during storage, transportation and mixing with feed; the second layer coating can also enhance the water-proof effect of the preparation and its resistance to rumen microorganisms.

[0057] (3) The oil in the core can not only reduce the use of water during granulation, but also give the formulation a certain sustained-release effect;

[0058] (4) The preparation method is simple and easy to operate, and can achieve continuous production, making it easy to promote and apply. Attached Figure Description

[0059] Figure 1 This is a process flow diagram of a rumen-transfer preparation method in one example of this application. Detailed Implementation

[0060] The following detailed description, in conjunction with specific embodiments, further illustrates the rumen-protected formulation, its preparation method, and its application. This application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of this application.

[0061] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of this application.

[0062] In this article, "one or more" refers to any one, two or more of the listed items.

[0063] In this application, terms such as "first aspect" and "second aspect" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or quantity, nor should they be construed as implicitly indicating the importance or quantity of the indicated technical features. Moreover, terms such as "first" and "second" serve only as a non-exhaustive enumeration and should be understood not to constitute a closed limitation on quantity.

[0064] In this application, the technical features described in an open-ended manner include both closed technical solutions consisting of the listed features and open technical solutions that include the listed features.

[0065] In this application, numerical ranges are referred to as continuous unless otherwise specified, and include the minimum and maximum values ​​of the range, as well as every value between the minimum and maximum values. Furthermore, when the range refers to integers, it includes every integer between the minimum and maximum values ​​of the range. Additionally, when multiple ranges are provided to describe a feature or characteristic, the ranges may be merged. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges to which they are incorporated.

[0066] Unless otherwise specified, the percentage content mentioned in this application refers to mass percentage for solid-liquid mixtures and solid-phase-solid mixtures, and volume percentage for liquid-phase-liquid mixtures.

[0067] Unless otherwise specified, all percentage concentrations mentioned in this application refer to the final concentration. The final concentration refers to the proportion of the added component in the system after the addition of that component.

[0068] Unless otherwise specified, the temperature parameters in this application may be either constant temperature processing or processing within a certain temperature range. The constant temperature processing allows for temperature fluctuations within the precision range controlled by the instrument.

[0069] In this application, room temperature generally refers to 4℃~30℃, and more preferably 20±5℃.

[0070] The first aspect of this application provides a method for preparing a rumen-protected preparation, the process flow diagram of which is shown below. Figure 1 As shown, it includes the following steps:

[0071] S1: Nutrients, oils, emulsifiers, and water are subjected to a first emulsification to prepare an oil-in-water (O / W) emulsion system;

[0072] S2: Granulation is performed using the oil-in-water emulsion system to prepare the core.

[0073] S3: Take another nutrient, oil, emulsifier, and water for a second emulsification to prepare a water-in-oil (W / O) emulsion system;

[0074] S4: The water-in-oil emulsion system is coated onto the surface of the core to prepare the first coating layer;

[0075] S5: Take another oil and melt it, then coat the surface of the first coating layer with the melted oil to prepare the second coating layer.

[0076] Understandably, the numbers S1 to S5 above are only used to more clearly describe the implementation scheme of this application and should not be regarded as a restriction on the order of the steps of this application.

[0077] In some of these examples, the nutrient is a water-soluble nutrient. Without limitation, the nutrient is one or more of glucose, choline, lysine, methionine, and niacin.

[0078] Specifically, steps S1 to S2 are the steps for preparing the core.

[0079] In some examples, the mass ratio of the emulsifier, the oil, and the nutrient is (1–10):(3–38):100. Specifically, this mass ratio includes, but is not limited to: 1:38:100, 10:38:100, 5:25:100, 1:3:100, 2:10:100, 3:10:100, 4:20:100, 2.3:9.6:100, 2.1:10.5:100, 3.2:13.2:100, 3.25:14.5:100, or a range between any two of the foregoing. Further, the mass ratio of the emulsifier, the oil, and the nutrient is (1–4):(7–18):100.

[0080] Understandably, the water refers to the water added when dissolving the aqueous phase substances such as nutrients during the preparation of the oil-in-water emulsion system and / or the water contained in the aqueous formulation raw materials. Without limitation, the mass ratio of the water to the nutrients can be (25–100):100.

[0081] Understandably, in the core, the emulsifier is an oil-in-water emulsifier. In some examples, in the core, the emulsifier is one or more of polyoxyethylene (8) stearate, polyoxyethylene (20) glyceryl stearate, polyoxyethylene sorbitan esters, and fatty acid salts. Without limitation, polyoxyethylene sorbitan esters may include, for example, one or more of Tween 20, Tween 40, Tween 60, Tween 65, and Tween 80, and fatty acid salts may include, for example, one or more of potassium, sodium, and calcium salts.

[0082] In some of these examples, the oil is a fatty acid having 14 or more carbon atoms; further optionally, the oil is one or more of stearic acid, soybean oil, rapeseed oil, sunflower oil, cottonseed oil, rice bran oil, corn oil, peanut oil, coconut oil, hydrogenated palm oil, rice bran wax, beeswax, and carnauba wax.

[0083] In some of these examples, the preparation of the core includes the following steps:

[0084] The water and the nutrients are mixed at a temperature of 60°C to 80°C to prepare an aqueous phase.

[0085] The emulsifier is mixed with the molten oil to prepare an oil phase;

[0086] The oil phase is added to the aqueous phase and emulsified to prepare the oil-in-water emulsion system.

[0087] Understandably, the mixing process dissolves and clarifies the materials.

[0088] Without restriction, emulsification is performed using shear emulsification to ensure the emulsion is homogeneous and stable.

[0089] Furthermore, the preparation of the aqueous phase also includes the step of adding a thickener. The thickener can increase the stability and viscosity of the emulsion, and increased emulsion viscosity can increase the particle size during granulation.

[0090] In some of these examples, the thickener includes one or more of xanthan gum, gum arabic, pectin, acid-modified starch, sodium carboxymethyl cellulose, and hydroxypropyl methylcellulose.

[0091] In some examples, the mass ratio of the thickener to the nutrient is (0.5–7):100. Specifically, this mass ratio includes, but is not limited to: 0.5:100, 1:100, 1.2:100, 1.3:100, 2:100, 2.75:100, 3:100, 4:100, 5:100, 6:100, 7:100, or a range between any two of the foregoing. Further, the mass ratio of the thickener to the nutrient is (1–4):100.

[0092] In some of these examples, the granulation method is spray granulation.

[0093] Furthermore, the conditions for spray granulation include: granulation temperature of 10℃~25℃, feed flow rate of 600kg / h~1200kg / h, and air humidity of 0%~5%.

[0094] Specifically, the granulation temperature includes, but is not limited to: 10℃, 13℃, 15℃, 17℃, 18℃, 20℃, 23℃, 25℃, or any range between the two. Further, the granulation temperature is 15℃~20℃.

[0095] Specifically, the feed flow rate includes, but is not limited to: 600 kg / h, 700 kg / h, 800 kg / h, 900 kg / h, 1000 kg / h, 1100 kg / h, 1200 kg / h, or any two of the foregoing. Further, the feed flow rate is 800 kg / h to 1000 kg / h.

[0096] Specifically, the intake air humidity includes, but is not limited to, 0%, 1%, 2%, 3%, 4%, 5%, or any two of the foregoing. Further, the intake air humidity is 0% to 3%.

[0097] In some examples, a drying step is included after granulation. Further, the drying conditions include a temperature of 40°C to 50°C and a time of 30 to 60 minutes. Fluidized bed drying can be used without limitation.

[0098] Specifically, the temperature includes, but is not limited to: 40°C, 41°C, 42°C, 43°C, 44°C, 45°C, 46°C, 47°C, 48°C, 49°C, 50°C, or any range between the two mentioned above.

[0099] Specifically, the time includes, but is not limited to: 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, or any range between the two. Further, the time is 40 min to 50 min.

[0100] Specifically, steps S3 to S4 are the steps for preparing the first coating layer.

[0101] In some examples, the mass ratio of the oil, the emulsifier, and the nutrient is (100–233):(1.5–12):100. Specifically, this mass ratio includes, but is not limited to: 100:1.5:100, 133:8:100, 233:12:100, 150:8:100, 170:6:100, 200:8:100, 122:5.3:100, 126:5.6:100, 166.7:7.5:100, 210:9:100, or any range between the foregoing. Further, the mass ratio of the oil, the emulsifier, and the nutrient is (115–223):(3–10):100.

[0102] Understandably, the water refers to the water added when dissolving the aqueous phase substances such as nutrients during the preparation of the water-in-oil emulsion system and / or the water contained in the aqueous formulation raw materials. Without limitation, the mass ratio of the water to the nutrients can be (25–100):100.

[0103] Understandably, in the first coating layer, the emulsifier is a water-in-oil emulsifier. In some examples, the emulsifier in the first coating layer is one or more of mono- and diglycerides, glyceryl monostearate, glyceryl acetate, glyceryl lactate, propylene glycol esters, stearoyl lactate, and sorbitan esters. Examples of sorbitan esters include, for instance, one or more of Span 20, Span 40, Span 60, Span 65, and Span 80.

[0104] In some examples, the oil in the first coating is a fatty acid having 14 or more carbon atoms; further optionally, the oil is one or more of stearic acid, tristearate, coconut oil, hydrogenated palm oil, beeswax, and carnauba wax.

[0105] In some of these examples, preparing the first coating layer includes the following steps:

[0106] The water and the nutrients are mixed at 60°C to 80°C to prepare an aqueous phase;

[0107] The emulsifier is mixed with the molten oil to prepare an oil phase;

[0108] The aqueous phase is added to the oil phase and emulsified to prepare the water-in-oil emulsion system;

[0109] The water-in-oil emulsion system is coated onto the surface of the core at a temperature of 30℃ to 60℃, and then cooled to prepare the first coating layer.

[0110] Understandably, the mixing process dissolves and clarifies the materials.

[0111] Without restriction, emulsification is performed using shear emulsification to ensure the emulsion is homogeneous and stable.

[0112] Specifically, step S5 is the step of preparing the second coating layer.

[0113] In some examples, during the step of preparing the second coating, the oil is a fatty acid having 14 or more carbon atoms. Further optionally, the oil is one or more of stearic acid, tristearate, coconut oil, hydrogenated palm oil, beeswax, and carnauba wax. Without limitation, during the preparation of the second coating, the oil is heated to 80°C–100°C to melt. Understandably, the trans fatty acid content in the oil should be less than 1%.

[0114] In some examples, the preparation of the second coating includes the following steps: applying molten grease to the surface of the first coating at a temperature of 40°C to 80°C.

[0115] Other examples of this application provide rumen-protected formulations prepared by the methods described above.

[0116] In some examples, the total weight percentage of the nutrients accounts for 40% to 70% of the total weight of the rumen-protected preparation. Specifically, the total weight percentage of the nutrients includes, but is not limited to: 40%, 43%, 45%, 47%, 50%, 53%, 55%, 57%, 60%, 63%, 65%, 67%, 70%, or any range between the foregoing. Further, the total weight percentage of the nutrients, based on the total weight of the rumen-protected preparation, is 45% to 67%.

[0117] In some examples, the particle size of the rumen-protected formulation is 0.8 mm to 1.4 mm. Specifically, the particle size includes, but is not limited to, 0.8 mm, 0.9 mm, 1.0 mm, 1.1 mm, 1.2 mm, 1.3 mm, 1.4 mm, or any range between the foregoing. Further, the particle size is 0.9 mm to 1.3 mm.

[0118] In some examples, the moisture content (by weight) of the rumen-protected preparation is 0-3%. Specifically, the moisture content includes, but is not limited to, 0, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, or any range between the foregoing. Further, the moisture content is 0-2.5%.

[0119] Other examples of this application provide the use of the rumen-protected preparations described above in the preparation of animal diets. Further, the animal is a rumen-containing rumen. Even further, the animal is a dairy cow. Without limitation, the rumen-protected preparations are added as feed additives to the animal's diet.

[0120] The raw materials and reagents involved in the following specific embodiments can be obtained commercially or prepared by those skilled in the art using known methods.

[0121] Example 1:

[0122] a) Mix 520 kg of glucose and 7 kg of acid-modified starch evenly, then add 150 kg of purified water at 75℃~80℃ and stir in an emulsifying stirred tank to obtain an aqueous phase; weigh 50 kg of stearic acid and melt it in a melting oil pot, then add 12 kg of Tween 80 until the Tween 80 is completely dissolved to obtain an oil phase; add the oil phase to the aqueous phase and shear at 5 m / s for 30 min to obtain an emulsion, then granulate it in a spray granulator at a granulation temperature of 18℃, a feed flow rate of 800 kg / h, and an inlet air humidity of 3%; then dry it in a fluidized bed at 45℃ for 45 min to obtain solid spherical glucose core granules with a moisture content of 2.3% and a particle size of 0.6 mm~1.0 mm.

[0123] b) Dissolve 150 kg of glucose in 41 kg of hot water at 75℃~80℃ to obtain a glucose solution; add 8 kg of emulsifier glyceryl monostearate to 183 kg of molten glyceryl tristearate, stir and dissolve to obtain a clear and transparent oil phase, then add the glucose solution to the oil phase, shear and emulsify for 30 min to obtain a one-time coated emulsion; add the glucose core particles obtained in step a to a hot melt coating machine and spray the above one-time coated emulsion at 45℃ for the first layer of coating, cool the discharged material to room temperature to obtain particles with a particle size of 0.8 mm~1.2 mm and a moisture content of 2.0%.

[0124] c) 70 kg of hydrogenated palm oil was melted at 90°C and used as an outer coating liquid to spray onto the surface of the particles obtained in step b) at 55°C for a second coating layer, resulting in rumen-protected glucose particles with a particle size of 0.9 mm to 1.3 mm, a glucose content of 66.0%, and a moisture content of 1.5%.

[0125] The particle size was measured using a Malvern particle size analyzer, the glucose content was measured according to GB 5009.8-2016 "Determination of fructose, glucose, sucrose, maltose and lactose in food", and the moisture content was measured using the 105℃ oven drying method.

[0126] Example 2:

[0127] a) Mix 420 kg of glucose with 5 kg of gum arabic evenly, add 110 kg of purified water at 75℃~80℃ and stir in an emulsifying stirring tank to obtain an aqueous phase; weigh 44 kg of soybean oil, add 9 kg of polyoxyethylene (20) stearic acid glycerol and stir until completely dissolved to obtain an oil phase; add the oil phase to the aqueous phase and shear at 5 m / s for 30 min to obtain an emulsion, then granulate in a spray granulator at a granulation temperature of 15℃, a feed flow rate of 900 kg / h, and an air humidity of 1%; then dry in a fluidized bed at 40℃ for 40 min to obtain solid spherical glucose core particles with a moisture content of 1.2% and a particle size of 0.6 mm~1.0 mm.

[0128] b) Dissolve 180 kg of glucose in 50 kg of hot water at 75℃~80℃ to obtain a glucose solution; add 10 kg of lactic acid fatty acid glyceride to 227 kg of molten carnauba wax, stir and dissolve to obtain a clear and transparent oil phase, then add the glucose solution to the oil phase, shear and emulsify for 30 min to obtain a one-time coated emulsion; add the glucose core particles obtained in step a to a hot melt coating machine and spray the above one-time coated emulsion at 60℃ for inner coating, cool the discharged material to room temperature to obtain particles with a particle size of about 0.8 mm~1.2 mm and a moisture content of 1.0%.

[0129] c) 105 kg of carnauba wax was melted at 90°C and used as an outer coating liquid to spray onto the surface of the particles obtained in step b) at 78°C to obtain rumen-protected glucose particles with a particle size of about 0.9 mm to 1.3 mm, a glucose content of 59.6%, and a moisture content of 0.7%.

[0130] Example 3:

[0131] a) Add 6 kg of sodium carboxymethyl cellulose and 507 kg of 75% (mass percentage) choline aqueous solution to an emulsifying stirred tank, heat and stir at 75℃~80℃ until completely dissolved to obtain an aqueous phase; weigh 50 kg of carnauba wax and dissolve it in an oil melting pot, add 12 kg of sodium fatty acid until the sodium fatty acid is completely dissolved to obtain an oil phase; add the oil phase to the aqueous phase, shear at 5 m / s for 30 min to obtain an emulsion, then granulate it in a spray granulator at a granulation temperature of 20℃, a feed flow rate of 1000 kg / h, and an inlet air humidity of 2%; then dry it in a fluidized bed at 50℃ for 45 min to obtain solid spherical choline core particles with a moisture content of 2.9% and a particle size of approximately 0.6 mm~1.0 mm.

[0132] b) Add 9 kg of glyceryl monostearate to 200 kg of molten beeswax, stir to dissolve and obtain a clear and transparent oil phase, then add 160 kg of 75% (mass percentage) choline aqueous solution preheated to 75℃~80℃, and shear emulsify for 30 min to obtain a one-time coated emulsion; add the choline core particles obtained in step a to a hot melt coating machine and spray the above one-time coated emulsion at 55℃ for inner coating, and cool the discharged material to room temperature to obtain particles with a particle size of about 0.8 mm~1.2 mm and a moisture content of 2.5%.

[0133] c) 132 kg of beeswax was melted at 90°C and used as an outer coating liquid to spray onto the surface of the particles obtained in step b) at 60°C to obtain rumen-coated choline particles with a particle size of about 0.9 mm to 1.3 mm, a choline content of 53.8%, and a moisture content of 2.2%.

[0134] Example 4:

[0135] a) Add 11 kg of acid-modified starch to 800 kg of 50% (mass percentage) L-lysine aqueous solution and stir at 75℃~80℃ until completely dissolved to obtain an aqueous phase; weigh 58 kg of corn oil and add 13 kg of sodium fatty acid and stir until completely dissolved to obtain an oil phase; add the oil phase to the aqueous phase and shear at 5 m / s for 30 min to obtain an emulsion, then granulate in a spray granulator at a granulation temperature of 15℃, a feed flow rate of 800 kg / h, and an inlet air humidity of 1%; then dry in a fluidized bed at 50℃ for 50 min to obtain solid spherical core particles with a moisture content of 1.5% and a particle size of approximately 0.6 mm~1.0 mm.

[0136] b) Add 9 kg of mono- and diglycerides to 210 kg of molten hydrogenated palm oil, stir to dissolve and obtain a clear and transparent oil phase, then add 200 kg of a 50% (mass percentage) L-lysine aqueous solution preheated to 75℃~80℃, and shear emulsify for 30 min to obtain a one-time coated emulsion; add the lysine core particles obtained in step a to a hot melt coating machine and spray the above one-time coated emulsion at 50℃ for inner coating, and cool the discharged material to room temperature to obtain particles with a particle size of about 0.8 mm~1.2 mm and a moisture content of 1.3%.

[0137] c) 125 kg of hydrogenated palm oil was melted at 90°C and used as an outer coating liquid to spray onto the surface of the particles obtained in step b) at 55°C to obtain rumen-protected lysine particles with a particle size of about 0.9 mm to 1.3 mm, a lysine content of 53.5%, and a moisture content of 1.0%.

[0138] Comparative Example 1:

[0139] This comparative example provides rumen-passed glucose granules, prepared using a spray granulation method, with the following steps:

[0140] a) Mix 510 kg of anhydrous glucose and 10 kg of light calcium carbonate, then pour the mixture into 450 kg of completely melted solid vegetable oil. Homogenize the mixture using a homogenizer, keeping the material temperature between 90°C and 100°C. Set aside for later use.

[0141] b) Through condensation spray granulation technology, the material is passed through a centrifugal atomizer to form regular spherical droplets. The particles solidify after contacting low-temperature air of 0℃~20℃ in the tower, forming regular spherical particles.

[0142] c) Screening for 60-14 mesh particles and mixing with 1.5% silica yields rumen-passed glucose particles with a glucose content of approximately 50%.

[0143] Comparative Example 2:

[0144] This comparative example provides rumen-protected glucose granules, prepared by extrusion granulation followed by coating, with the following steps:

[0145] a) Mix 600 kg of glucose, 50 kg of silicon dioxide and 2.65 kg of sodium carboxymethyl cellulose, add 80 kg of water, adjust the mixture to a granulation state, granulate it with a granulator, then shot blast it with a shot blasting machine, and dry it to obtain glucose granules.

[0146] b) Dissolve 340 kg of hydrogenated palm oil at 90 °C and use it as a coating solution to spray onto the surface of the particles obtained in step a) to coat them, resulting in rumen-coated glucose particles with a glucose content of approximately 60%.

[0147] Test example:

[0148] (1) Determination of rumen-passing rate of rumen-passing preparations

[0149] The rumen-passing rate of the rumen-passing preparation samples in the pilot and comparative examples was determined using a fistula-guided cattle test. The experiment was conducted as follows: A nylon filter cloth with 50 μm mesh was used to prepare 12 cm × 8 cm (length × width) nylon bags. 10.0 g of the rumen-passing preparation sample was accurately weighed into each nylon bag, and the bag opening was secured with a rubber band. Three replicates were set up for each cow at each time point. The sample was administered before morning feeding and cultured for 4 h, 8 h, 12 h, 16 h, 24 h, 36 h, and 48 h. The rumen-passing rate of the sample in the dairy cows was calculated. The content of the corresponding nutrients in the feed additive was determined using the residual iodine method according to national standards.

[0150] The test results are shown in Table 1 below.

[0151] Table 1. Rumen-crossing rate (%) of rumen-crossing preparations

[0152]

[0153] As shown in Table 1, compared with Comparative Examples 1 and 2, the rumen passage rate of the samples in Examples 1 to 4 was significantly increased.

[0154] (2) Determination of small intestinal digestibility of rumen-passed preparations

[0155] The small intestinal digestibility of the rumen-protected formulations in the examples and comparative examples was determined using a semi-in vitro three-step method, as follows:

[0156] After the rumen-processed preparation sample underwent 16 hours of fermentation and degradation in the rumen, a certain amount of non-degraded rumen residue was collected. 1g of the residue was placed in a nylon bag (5cm × 10cm), and a maximum of 12 bags were incubated in a 2L Erlenmeyer flask at a time. The Erlenmeyer flask contained 2L of hydrochloric acid solution with pH = 1.9 containing 1g / L pepsin (P-7012, Sigma-Aldrich, USA, activity ≥2500U / mg prot, potency 100%), preheated beforehand. The mixture was incubated at a constant temperature of 39℃ for 1 hour. After incubation, the nylon bags were removed, drained, and rinsed with tap water until clear. They were then placed in a small intestinal fistula for 24 hours, rinsed thoroughly, and dried at 40℃ to constant weight. The release rate of the sample in the small intestine was determined based on the rate of nutrient loss from the feed in the nylon bags.

[0157] Small intestinal release rate = (Content of corresponding nutrients in the rumen-protected preparation - Content of corresponding nutrients in the residue after enzymatic hydrolysis) / Content of corresponding nutrients in the rumen-protected preparation × 100%

[0158] Table 2. Small intestinal release rate (%) of rumen-protected preparations

[0159] Small intestinal release rate Example 1 97.85±1.38 Example 2 94.22±1.53 Example 3 90.09±1.01 Example 4 91.32±1.30 Comparative Example 1 96.78±1.01 Comparative Example 2 89.57±1.16

[0160] As shown in Table 2, compared with Comparative Examples 1 and 2, the sample of Example 1 has a small intestinal release rate that is comparable to or even better. Although the small intestinal release rates of Examples 2, 3 and 4 are lower than those of Comparative Example 1, they are still relatively high and can meet the required bioavailability and therapeutic effect.

[0161] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0162] The embodiments described above are merely illustrative of several implementation methods of this application, intended to facilitate a detailed understanding of the technical solutions of this application, but should not be construed as limiting the scope of protection of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the scope of protection of this application. It should be understood that technical solutions obtained by those skilled in the art based on the technical solutions provided in this application through logical analysis, reasoning, or limited experimentation are all within the scope of protection of the appended claims. Therefore, the scope of protection of this patent application should be determined by the content of the appended claims, and the specification can be used to interpret the content of the claims.

Claims

1. A method for preparing a rumen-exposed preparation, characterized in that, Includes the following steps: Nutrients are emulsified with oils, emulsifiers, and water to prepare an oil-in-water emulsion system. The core is prepared by granulation using the oil-in-water emulsion system described above; Nutrients were emulsified with oils, emulsifiers, and water to prepare a water-in-oil emulsion system. The water-in-oil emulsion system is coated onto the surface of the core to prepare a first coating layer. Separately, melt the oil and coat the surface of the first coating layer with the melted oil to prepare the second coating layer. The preparation of the core includes the following steps: The water and the nutrients are mixed at a temperature of 60℃~80℃ to prepare an aqueous phase; The emulsifier is mixed with the molten oil to prepare an oil phase; The oil phase is added to the aqueous phase and emulsified to prepare the oil-in-water emulsion system; The preparation of the first coating layer includes the following steps: The water and the nutrients are mixed at 60°C to 80°C to prepare an aqueous phase. The emulsifier is mixed with the molten oil to prepare an oil phase; The aqueous phase is added to the oil phase and emulsified to prepare the water-in-oil emulsion system; The water-in-oil emulsion system is coated onto the surface of the core at a temperature of 30℃~60℃ and then cooled to prepare the first coating layer.

2. The method for preparing the rumen-protected preparation according to claim 1, characterized in that, The nutrients are one or more of glucose, choline, lysine, methionine, and niacin.

3. The method for preparing the rumen-protected preparation according to claim 1, characterized in that, The steps for preparing the core have at least one of the following characteristics: (1) The mass ratio of the emulsifier, the oil and the nutrient is (1~10):(3~38):100; (2) The mass ratio of the water to the nutrients is (25~100):100; (3) The emulsifier is one or more of polyoxyethylene (8) stearate, polyoxyethylene (20) stearate glycerol, polyoxyethylene sorbitan esters and fatty acid salts; (4) The oil is a fatty acid with 14 or more carbon atoms.

4. The method for preparing the rumen-protected preparation according to claim 3, characterized in that, The steps for preparing the core have at least one of the following characteristics: (1) The mass ratio of the emulsifier, the oil and the nutrient is (1~4):(7~18):100; (2) The oil is one or more of the following: stearic acid, soybean oil, rapeseed oil, sunflower oil, cottonseed oil, rice bran oil, corn oil, peanut oil, coconut oil, hydrogenated palm oil, rice bran wax, beeswax and carnauba wax.

5. The method for preparing the rumen-protected preparation according to claim 1, characterized in that, The preparation of the aqueous phase also includes the step of adding a thickener; the thickener includes one or more of xanthan gum, gum arabic, pectin, acid-modified starch, sodium carboxymethyl cellulose and hydroxypropyl methyl cellulose.

6. The method for preparing the rumen-crossed preparation according to claim 5, characterized in that, The mass ratio of the thickener to the nutrient is (0.5~7):

100.

7. The method for preparing the rumen-protected preparation according to claim 5, characterized in that, The mass ratio of the thickener to the nutrient is (1~4):

100.

8. The method for preparing the rumen-protected preparation according to claim 1, characterized in that, The granulation method is spray granulation.

9. The method for preparing the rumen-crossed preparation according to claim 8, characterized in that, The conditions for spray granulation include: granulation temperature of 10℃~25℃, feed flow rate of 600kg / h~1200kg / h, and air humidity of 0%~5%.

10. The method for preparing the rumen-protected preparation according to claim 1, characterized in that, The granulation process also includes a drying step. The drying conditions include a temperature of 40℃~50℃ and a time of 30min~60min.

11. The method for preparing the rumen-crosslinked preparation according to any one of claims 1 to 10, characterized in that, The steps for preparing the first coating layer have at least one of the following characteristics: (1) The mass ratio of the oil, the emulsifier and the nutrient is (100~233):(1.5~12):100; (2) The mass ratio of the water to the nutrients is (25~100):100; (3) The emulsifier is one or more of the following: monoglycerides and diglycerides, glyceryl monostearate, glyceryl acetate, glyceryl lactate, propylene glycol esters, stearoyl lactate, and sorbitan esters; (4) The oils mentioned are fatty acids with 14 or more carbon atoms.

12. The method for preparing the rumen-crossed preparation according to claim 11, characterized in that, The steps for preparing the first coating layer have at least one of the following characteristics: (1) The mass ratio of the oil, the emulsifier and the nutrient is (115~223):(3~10):100; (2) The oil is one or more of stearic acid, tristearate, coconut oil, hydrogenated palm oil, beeswax and carnauba wax.

13. The method for preparing the rumen-crosslinked preparation according to any one of claims 1 to 10, characterized in that, In the step of preparing the second coating, the oil is a fatty acid having 14 or more carbon atoms.

14. The method for preparing the rumen-crossed preparation according to claim 13, characterized in that, The oil is one or more of stearic acid, tristearate, coconut oil, hydrogenated palm oil, beeswax, and carnauba wax.

15. The method for preparing the rumen-crosslinked preparation according to any one of claims 1 to 10, characterized in that, The preparation of the second coating includes the following steps: At temperatures of 40°C to 80°C, the molten grease is coated onto the surface of the first coating layer.

16. A rumen-protected preparation obtained by the preparation method according to any one of claims 1 to 15.

17. The rumen-crossing preparation according to claim 16, characterized in that, It has at least one of the following characteristics: (1) The total weight of the nutrients accounts for 40% to 70% of the total weight of the rumen-protected preparation; (2) The particle size of the rumen-exposed preparation is 0.8 mm to 1.4 mm; (3) The moisture content of the rumen-protected preparation is 0-3%.

18. The rumen-crossing preparation according to claim 17, characterized in that, The total weight of the nutrients accounts for 45% to 67% of the total weight of the rumen-protected preparation.

19. The use of the rumen-exposed preparation according to any one of claims 16 to 18 in the preparation of animal diets.

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