Process for producing encapsulated amino acids for ruminants

Abstract

To provide a process of encapsulating or coating amino acid particles for producing an encapsulated amino acid feed product for ruminant animals.SOLUTION: The encapsulated amino acid feed product comprises a substantially uniform dust free pastille granules. When the encapsulated amino acid feed product is fed to a ruminant animal, the product delivers high amounts of absorbable amino acid to the animal for direct nourishment, the amino acid being not substantially fermented in the rumen of the animal. In an aspect, the process is a low-cost, high capacity, continuous process that produces a composition comprising greater than 50 wt.% of a nourishing amino acid. The superior handling quality of the pastille granules allows for their use in further formulation of animal feeds, where homogeneous distribution of nutrients throughout a mixed feed is desired.SELECTED DRAWING: None

Description

[Technical Field]

[0001]

[01] The present invention relates to a process for producing a composition that delivers high amounts of absorbable amino acids for direct nutritional feeding to ruminants, and the composition produced thereby. [Background technology]

[0002]

[02] Ruminants have evolved a fermentation process in their large forestomach to digest feedstuffs that are normally indigestible through the digestion process of mammalian hydrolytic enzymes. The beneficial process associated with fermenting cellulosic and other feedstuffs is that they provide the animals with nutritional end-products such as microbial protein, volatile fatty acids, and vitamins. However, high-quality proteins and free amino acids can be fermented in the ruminant's first stomach (also called the "rumen"), reducing their value. In particular, free amino acids, when added directly to the diet, are fermented to ammonia and volatile fatty acids, which are far less valuable to the animal than amino acids. Therefore, fermentation of feedstuffs, particularly amino acids, in the rumen presents a challenge in formulating diets that precisely provide the essential amino acids needed for ruminant growth and maximize milk production.

[0003]

[03] Various compositions and methods for controlling the delivery and release of amino acids have been tested. Some of these approaches have shown promise and commercial value. However, developing and implementing high-throughput processing methods to consistently produce rumen-protected amino acids for subsequent release in the small intestine has proven difficult. Traditional coating technologies and methods for producing encapsulated products are expensive, and the resulting product quality may not justify the cost. Typically, the functional effect of traditional coating materials is far removed from protecting amino acids from fermentation by rumen microorganisms. While protective, certain coatings have not been approved as safe for animal feed applications.

[0004]

[04] A variety of conventional protective barriers have been utilized. An effective barrier mechanism limits the exposure of feed amino acids as they pass through the rumen while simultaneously allowing rapid nutrient release upon exposure to the digestive process in the acidic enzyme compartments of the digestive tract. Amino acids such as methionine and lysine, which are predicted to be most functionally limiting, are of great commercial interest. Because each amino acid has unique chemical and physical characteristics, barrier technology must be tailored to the specific characteristics of the amino acid. Encapsulating amino acids in a protective matrix or outer shell adds cost and necessarily dilutes the amino acids provided by the feed product. Sufficient amino acid concentration, technical delivery, and cost-effective manufacturing techniques in feed products are not achieved with conventional approaches. Summary of the Invention

[0005]

[05] One aspect of the present disclosure provides a manufacturing process that overcomes the limitations of conventional manufacturing techniques and surprisingly produces a composition that, when fed to a ruminant, can deliver high amounts of absorbable amino acids for direct nutritional feeding to the animal. In one aspect, the process includes deposition and pastillation techniques that produce a composition containing greater than 50% by weight of amino acids for nutritional feeding. The process produces uniformly sized particles (i.e., encapsulates or pastilles) in a continuous process that is low cost and has high production capacity.

[0006]

[06] In one aspect, the process includes encapsulating or coating an animal feed ingredient, the process including combining an emulsifier and a coating agent to form a coating mixture, and disposing the coating mixture over particles of the animal feed ingredient, thereby encapsulating or coating the animal feed ingredient.

[0007]

[07] In one aspect of the present disclosure, a process includes mixing and heating an emulsifier with hydrogenated vegetable oil to form a coating mixture, and mixing the coating mixture with amino acid particles to form a slurry. The process can further include heating the slurry to form a molten product. The process can further include dripping the molten product onto a belt cooler as a substantially uniform, dust-free pastille granule using a drop granulator. [Brief explanation of the drawings]

[0008]

[08] The present invention may be more fully understood and advantageously obtained by reference to the following description taken in conjunction with the accompanying drawings, in which like reference numerals represent like features, and in which:

[0009] [Figure 1]

[09] Figure 1 illustrates a flow diagram of a process according to an embodiment of the present disclosure. [Figure 2]

[10] FIG. 2 illustrates a further embodiment of the drop granulator more generally shown in FIG. [Figure 3]

[11] Figure 3 illustrates the landing of product through the opening of a drop granulator, shown more generally in Figure 1, onto a cooling belt. [Figure 4]

[12] Figure 4 shows viscosity curves as a function of shear rate at 85°C in the presence of emulsifiers (GMS - glycerol monostearate, SMS - sorbitan monostearate, 3-1-S - triglycerol monostearate, and 10-1-S - decaglycerol monostearate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, the compositions comprising a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier. [Figure 5]

[13] Figure 5 shows viscosity curves as a function of shear rate at 85°C in the presence of emulsifiers (SMS - sorbitan monostearate, SML - sorbitan monolaurate, and SMO - sorbitan monooleate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, the compositions comprising a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier. [Figure 6]

[14] Figure 6 shows the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (10-1-S -decaglycerol monostearate, Yelkin® SS lecithin from Archer Daniels Midland Company, or 6-2-S -hexaglycerol monostearate) for a composition comprising encapsulated lysine according to an embodiment of the present disclosure, the composition comprising a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier. [Figure 7]

[15] Figure 7 shows the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (Yelkin® SS lecithin or 10-1-S -decaglycerol monostearate from Archer Daniels Midland Company) for a composition comprising encapsulated lysine according to an embodiment of the present disclosure, the composition comprising a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 40 mesh sieve. [Figure 8]

[16] Figure 8 illustrates the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (Yelkin® SS lecithin or 10-1-S -decaglycerol monostearate from Archer Daniels Midland Company) for a composition comprising encapsulated lysine according to an embodiment of the present disclosure, the composition comprising a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl sieved through a 60 mesh screen. [Figure 9]

[17] Figure 9 illustrates the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (Yelkin® SS lecithin from Archer Daniels Midland Company) for compositions comprising encapsulated lysine according to an embodiment of the present disclosure, the compositions comprising either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 60 mesh sieve. [Figure 10]

[18] Figure 10 illustrates the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (Yelkin® SS lecithin from Archer Daniels Midland Company) for compositions comprising encapsulated lysine according to an embodiment of the present disclosure, the compositions comprising either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 100 mesh sieve. [Figure 11]

[19] Figure 11 illustrates the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (SMS - sorbitan monostearate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, the compositions comprising either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 60 mesh sieve. [Figure 12]

[20] Figure 12 illustrates the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (SMS - sorbitan monostearate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 100 mesh sieve. [Figure 13]

[21] Figure 13 illustrates the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (lecithin) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend, a 45:55 blend, or a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 40 mesh sieve. [Figure 14]

[22] Figure 14 illustrates the viscosity curve as a function of shear rate at 85°C in the presence of an emulsifier (10-1-S -decaglycerol monostearate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend, a 45:55 blend, or a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 40 mesh sieve. [Figure 15]

[23] Figure 15 illustrates the viscosity curve as a function of shear rate at 85°C for a composition comprising encapsulated lysine in the presence of an emulsifier (Yelkin® SS Lecithin or Yelkin® SS Lecithin with phytonutrient essential oil, i.e., thymol, or peppermint oil, or curcumin from Archer Daniels Midland Company), according to an embodiment of the present disclosure, the composition comprising a 49:50 blend of hydrogenated soybean oil and lysine, with 1% emulsifier and 1% wt:wt essential oil phytonutrient, and the lysine HCl was sieved through a 40 mesh sieve. [Figure 16]

[24] Figure 16 illustrates the viscosity curve as a function of shear rate at 85°C for a composition comprising encapsulated lysine in the presence of an emulsifier (SMS - sorbitan monostearate or a phytonutrient essential oil, i.e., SMS - sorbitan monostearate in combination with thymol or peppermint oil or curcumin) according to an embodiment of the present disclosure, the composition comprising a 49:50 blend of hydrogenated soybean oil and lysine with 1% emulsifier and 1% wt:wt of either the phytonutrient essential oil, and the lysine HCl was sieved through a 40 mesh sieve. [Figure 17]

[25] Figure 17 shows the effect of emulsifier / surfactant choice on lysine HCl content and ruminal stability (RUP). DETAILED DESCRIPTION OF THE INVENTION

[0010]

[26] Many conventional coating compositions incorporate lipids or fatty acids, which are hydrophobic and nutritionally acceptable substances, to provide a basis for withstanding the aqueous environment of the rumen. The challenge encountered here is that the melting points and densities of amino acids present as dry solids in the formulation are different from those of lipids. Because amino acids and lipids have different solubilities based on their opposing hydrophilic and hydrophobic properties, blending them together in the molten state can often result in phase separation of the slurry. This phase separation can occur not only in the bulk phase but also in the small microdomains of the fat crystal network. Amino acids can be included in the formulation either as salts (which add to the physical properties of particle distribution) or as "free" amino acids (which are often contained in aqueous solutions, exacerbating the challenges of hydrophobic and hydrophilic interactions). Separation of components within the matrix can lead to unevenness in the final product and reduced protection from the rumen environment. In one aspect of the present disclosure, the amino acid can be an amino acid that is beneficial to a ruminant animal when added to the animal's feed, including, but not limited to, lysine, methionine, histidine, choline, and any combination thereof.

[0011]

[27] In one aspect of the present disclosure, a novel technique is provided that overcomes the difficulties and limitations of conventional approaches. Experiments were designed and conducted to test specific characteristics of solid particles, emulsifiers, lipids, and the rheological properties of slurries prepared using a drop granulation process. Surprisingly, it was found that when performing drop granulation / droplet landing processing, the rheological parameters were well controlled and it was possible to incorporate a high percentage of solids into the slurry or melt product.

[0012]

[28] In one aspect of the present disclosure, a fluid slurry is provided for producing a uniform granulation that meets target specifications. A more precise understanding of the rheology allows for the selection of compositions containing amino acids, lipids, and emulsifiers (and adjustments for other additives, if desired).

[0013]

[29] Slurry viscosity increases with the solids content and the fineness of the added solids (i.e., amino acids). The inclusion of an emulsifier can reduce the surface tension at the solid / liquid interface, thereby reducing viscosity. Furthermore, the shear-thinning properties of slurries allow for higher solid loadings, thereby providing fluidity during processing. Similar fatty acid chain lengths and unsaturation levels in the "tails" of the emulsifier and fat used can also improve performance. It has generally been found that, for a given solid concentration and solid particle size, emulsifiers with larger "heads" can achieve greater viscosity reductions. Common emulsifiers with favorable properties commonly used in animal foods are sorbitan esters and lecithin (of which phosphatidylcholine is a component). Phosphatidylcholine is generally considered a beneficial component of lecithin because it is rich in choline, a B-complex vitamin involved in certain biological functions. The presence of emulsifiers in systems with extreme solubility parameters promotes lubrication of solids within the fat system by creating more nucleation sites, allowing for the loading of hydrophilic solids in the fat slurry at higher levels, producing a more homogeneous dispersion and resulting in more uniform granulation in the process.

[0014]

[30] Lecithin contains two fatty acid chains and a large phosphate ester head group. Lecithin has been described in the prior art for compositions and methods for producing encapsulated products for use in ruminant diets due to its favorable emulsifying properties. Lecithin is a well-described food emulsifier commonly used in chocolate production to reduce the viscosity of solid sugars, but is ineffective at improving yield properties. Polyglycerol polyricinoleate (PGPR) is a polyglycerol ester-based emulsifier often used in combination with lecithin to achieve viscosity and yield properties; the lecithin-PGPR combination exhibits synergistic interactions and is commonly used in chocolate production. Surprisingly, a single emulsifier, diglycerol ester, was found to rival the functionality of lecithin. Structurally similar emulsifiers, such as hexaglycerol distearate in addition to phospholipids, have similar functionality in controlling the rheological parameters of fat-lysine slurries. However, the larger polyglycerol (decaglycerol) was more effective than lecithin at controlling the viscosity of high solids slurries.

[0015]

[31] FIG. 1 illustrates a process flow diagram for a process according to an embodiment of the present disclosure. As shown in FIG. 1, a drop granulation system 100 includes a mixing vessel 2, a drop granulator 4, a belt cooler 6, and a bagging device 8. Raw materials 10 and a coating mixture 12 can be added to the mixing vessel 2 through a top opening 14. The raw materials 10 can include amino acids provided by an amino acid source 16. The coating mixture 12 can include a mixed emulsifier and coating agent and is provided by a coating mixture source 18. The raw materials 10 and the coating mixture 12 can be mixed in the mixing vessel 2 to form a slurry by rotating an impeller 20 about a vertical axis AA. The raw materials 10 and the coating mixture 12 can be heated in the mixing vessel 2 to produce a molten product 22. For example, the raw materials and the coating mixture can be heated 10° C. above the melting point of the fat. In an alternative embodiment (not shown in FIG. 1 ), the raw materials 10 and the coating mixture 12 can be heated together or separately before being mixed in the stirred tank 2, or can be heated after being mixed in the stirred tank 2. The molten product 22 can be withdrawn from the stirred tank 2 through a bottom opening 24 of the stirred tank 2. The molten product 22 can be pumped from the stirred tank 2 to the drop granulator 4 using a pump 26. In one embodiment, the molten product 22 can be passed through a filter 28 to remove undesirable large particles or agglomerates, such that a substantially uniform filtered molten product emerges from the filter 28 and is conveyed or delivered to the drop granulator 4.

[0016]

[32] The drop granulator 4 is configured to heat the filtered molten product 22 to maintain the flowability of the molten product 22 and form a granulation containing the encapsulated amino acids. The drop granulator 4 is configured to drop and land the substantially uniform, dust-free, drop granulated granules 30 (containing the encapsulated amino acid particles) onto the belt cooler 6 near the proximal end 32 of the belt cooler 6. In one embodiment, the substantially uniform, dust-free, drop granulated granules 30 can be substantially hemispherical in shape. In another embodiment, the substantially uniform, dust-free, drop granulated granules can have a substantially pyramidal shape (similar to a chocolate chip shape). In one embodiment, the aspect ratio (diameter:height) of the drop granulated granules is 1.5 to 2.5, about 1.7, or about 2.0 for a hemispherical shape. In another embodiment, the substantially uniform, dust-free drop-granulated granules can be substantially flat-sided spheres (similar to the shape of a hockey puck). The drop granulator 4 can be configured to produce a desired size of granules, e.g., a diameter (as viewed from above after the drop-granulated granules have dropped onto the belt cooler 6 and landed) ranging from 1 to 25 mm. The drop-granulated granules 30 can be collected from the distal end 34 of the belt cooler 6 and transported to a bagging facility 8, where the drop-granulated granules can be loaded into bags 36. The drop granulator 4 can be operated continuously for extended periods of time. Water can be pumped from a water tank 40 by a cooling water pump 38 to a cooler 42 and then to a cooling water sprayer 44 equipped with spray nozzles 46. Cooling water can be sprayed onto a bottom interface 48 of the belt cooler 6 through a spray nozzle 46 by a sprayer 44, thereby cooling the belt cooler 6 and the drop granulated granules 30 on the belt cooler 6. The sprayed water can be returned to the water tank 40. The belt cooler 6 can rotate around belt rollers 50 and 52. As shown in FIG. 1 , the belt roller 50 is located on the proximal side of the drop granulator 4, and the belt roller 52 is located on the distal side of the granulator 4.

[0017]

[33] The excellent handling properties of the drop-granulated granules allow them to be used for further incorporation into animal feeds where it is desirable to have a uniform distribution of nutrients throughout the final mixed feed.

[0018]

[34] Figure 2 illustrates a further embodiment of the drop granulator 4 more generally shown in Figure 1. As shown in Figure 2, the drop granulator 4 includes a product distribution pipe 200, a heat shield 204, a heated cylindrical stator 206, a heating medium 208, and a product distribution bar 210. The drop granulator 4 may also include a refeed bar 212. As discussed above, the drop granulator 4 is configured to drip and land substantially uniform, dust-free, drop granulated granules 30 (containing encapsulated amino acids) onto the belt cooler 6. The filtered molten product provided by the filter 28 (shown in Figure 1) is heated in the drop granulator 4 to maintain the flowability of the molten product 22. The molten product 22 drops through the product dispensing opening 202 to land on the belt cooler 6 as substantially uniform, dust-free drop granulated granules 30 (containing encapsulated amino acids). The cooling water spray nozzles 46 are configured to spray cold water onto the interface 48 to cool the belt cooler 6 and the drop granulated granules 30 that land on the belt cooler 6. The belt cooler 6 may include a belt roller 216. The belt roller 216 may be the same as or different from the belt rollers 50 and 52. The vertical distance between the belt cooler 6 and the drop granulator 4 can be adjusted by the roller 216 moving vertically relative to the drop granulator 4.

[0019]

[35] The heated cylindrical stator 206 may include hollow rollers 218. The heated cylindrical stator 206 may include a rotating perforated barrel 220 that rotates coaxially around the stator, causing droplets of the molten product 22 to fall and land as drop-granulated granules 30 across the operating width of the steel belt or belt cooler 6. A system of baffles and internal nozzles within the heated cylindrical stator 206 applies uniform pressure across the operating width of the belt cooler 6, resulting in uniform flow through all holes or product distribution openings 202 in the rotating perforated barrel 220. This ensures that each row of drop-granulated granules 30 from one end of the belt to the other is of uniform size.

[0020]

[36] The peripheral speed of the drop granulator 4 is synchronized with the belt speed, ensuring that the droplets land on the belt without deformation. Heat released during solidification and cooling is conducted by a stainless steel belt or belt cooler 6 to cooling water sprayed directly below it. This water is collected in a vessel, e.g., vessel 40, and returned to the water cooling system or cooler 42; the product or drop granulated granules 30 do not come into direct contact with water at any stage. The design of an effective drop granulation system takes into account many factors. For example, the minimum diameter of the granules depends on the diameter of the holes or product dispensing openings 202 in the rotating barrel 220, the density and viscosity of the product itself, the surface tension and mechanical acceleration of the droplets. Those skilled in the art will recognize that, in accordance with the present disclosure, the droplets should have sufficient weight and volume to drip and land on the steel belt or belt cooler 6, and the distance between the rotating outer barrel 220 and the steel belt can be adjusted to obtain an efficient process and the desired drop granulated granules 30.

[0021]

[37] Those skilled in the art will recognize that, following this disclosure, suitable process parameters and component placement can be further refined using custom-developed computer programs and / or trial runs using the specific product being processed.

[0022]

[38] Figure 3 illustrates the dripping of drop granulated granules 30 onto a belt cooler 6. As shown in Figure 3, drop granulated granules 30 drip onto the belt cooler 6 through product dispensing openings 202. Those skilled in the art having the benefit of this disclosure will recognize that suitable pin and / or needle structures can be used to deliver drop granulated granules 30 onto the belt cooler 6 through product dispensing openings 202.

[0023]

[39] In one embodiment, a product produced by any of the processes described herein is produced.

[0024]

[40] In another embodiment, the drop-granulated granules contain an amino acid, an emulsifier, and a coating agent. The drop-granulated granules have a roughly hemispherical shape with an aspect ratio (diameter / height) of 1.5 to 2.5.

[0025]

[41] The amino acid may be selected from the group consisting of lysine, histidine, methionine, choline, and any combination thereof. The emulsifier may be selected from the group consisting of lecithin, monoglyceride, sorbitan ester, polyglycerol, and combinations thereof. The coating agent may be selected from the group consisting of oil, fatty acid, and combinations thereof. The coating agent may be hydrogenated vegetable oil. The size of the drop-granulated granules may be 2.2 to 5.0 mm or 2.2 to 3.5 mm. The particle size of the amino acid may be 50 to 120 mesh or 80 to 110 mesh. The amino acid may be present in the drop-granulated granules at 25 to 85 wt%, 25 to 75 wt%, or 35 to 75 wt%.

[0026]

[42] In another embodiment, a method of feeding an animal comprises mixing the drip granulated granulate produced as described herein with animal feed ingredients to form an animal feed, and feeding the animal feed to an animal, which may be a ruminant.

[0027]

[43] In a further embodiment, a process for encapsulating amino acid particles includes mixing an emulsifier with a coating agent to form a coating mixture, mixing the coating mixture with amino acid particles to form a slurry, forming granulation with the slurry, and dripping the granulation onto a belt. The process can further include heating the coating mixture and / or cooling the granulation on the belt. [Example]

[0028]

[44] Other aspects of the processes and encapsulated products of the present disclosure are further described in conjunction with the following examples.

[0029] Example 1. Effect of lysine particle size and emulsifier usage on rumen integrity (viscosity as a differentiating feature)

[46] The following examples demonstrate viscosity as a differentiating feature in accordance with embodiments of the present disclosure. Tests were conducted to evaluate the equipment and handling for spray granulation in a spray cooling process. The purpose of these tests was to form approximately 1 mm prills and evaluate rumen integrity (stability) as affected by the amount and size of lysine and the choice of emulsifier. Lysine HCl in dry powder form was included at 50% of the slurry. The lysine HCl was either milled recharge, which has a broader particle size distribution, or sieved through a 40-mesh screen. The balance of the formulation was hydrogenated soybean or palm oil. During testing, 25 lb batches of slurry were formed using a rotating disk operating in a spray tower. The results are shown in Table 1.

[0030] [Table 1]

[0031]

[47] In this experiment, the yield of acceptable particle sizes was low, and ruminal stability was inferior compared to commercially available encapsulated products. Slurry mixability was particularly poor with broader-spectrum, coarser materials (i.e., <40 mesh lysine granules), resulting in a "gritty" slurry. Viscosity and flow became problematic above 50% solids, and slurry separation was observed. High emulsifier loading was required to achieve a flowability suitable for spray cooling at 50% solids. High emulsifier content can be detrimental to encapsulation. Its ability to hydrate particles results in a stable dispersion in an aqueous environment. However, the encapsulation process is also an important parameter for creating a ruminal-stable product.

[0032] Example 2. Evaluation of Lysine Formulations Across Processing Methods (Viscosity Affects Processing Method and Therefore Allows Control to Improve Product)

[49] A series of studies was conducted to evaluate processing techniques (jet granulation, fluidized-bed coating, extrusion, and drop granulation) and the interaction of composition with processing. Lysine hydrochloride (Lys HCl) with various particle size distributions (unsieved and sieved Lys HCl) was used in the formulations. Slurries containing 40 or 50% Lys HCl were blended, and a monoglyceride emulsifier (Alphadim® 90 SBK from Corbion) was added at between 0.5 and 5% by weight of the blend and heated to approximately 20°C above the melting point of the fat system. The remainder of the material consisted of fully hydrogenated soybean oil. The coating process utilized fully hydrogenated soybean oil plus emulsifier and sprayed onto the lysine granules. Samples of each prototype were incubated in the rumen of lactating dairy cows for 16 hours and then evaluated for ruminal stability. The results are shown in Table 2.

[0033] [Table 2]

[0034]

[50] Pellets produced by spray chilling prototypes became more spherical with increasing viscosity and particle size increased somewhat. Rumen stability improved with decreasing lysine content. Extrusion offered more freedom in formulating the lysine suspension and forming the particles, but fractures along the edges of the particles appeared to compromise rumen integrity. Fluidized bed processing provided better rumen integrity than spray chilling and comparable to extrusion.

[0035]

[51] Drop granulation processing resulted in excellent globule integrity, especially when the particle size of Lys HCl was controlled to <40 mesh. It was found that the viscosity could be adjusted sufficiently to allow drop granulation of high-solids suspensions to obtain granules with an average particle size greater than 2 mm. Increasing the amount of emulsifier in the composition did not improve the ruminal integrity of the granules; in fact, lower concentrations resulted in greater granule stability. For these high-solids fat slurry systems, it was found that the rheological properties are a function of the emulsifier, not the amount. However, significant tradeoffs exist between process, composition, physical properties such as particle size, rheology, and ruminal stability. This study demonstrated that by controlling viscosity through solid particle size and emulsifier amount, it is possible to process slurries with increased solid content to produce granules with excellent ruminal integrity. This study demonstrated that various processing techniques can be used to produce solid particles with varying degrees of ruminal integrity. However, it was concluded that among the processing techniques investigated, drip granulation appears to be the most promising. Furthermore, by precisely formulating the composition used in processing, the integrity of the granules after ruminal incubation exceeded 95%.

[0036] Example 3. Inclusion of functional additives in the composition further differentiates it and contributes to nutritional provision

[53] Animals face a variety of challenges in which commercial feeding practices can impair their health and well-being or result in poor nutritional status due to malabsorption or altered gastrointestinal function. Feed additives, particularly natural phytonutrients found in botanical and plant extracts, are often added to animals' feed to aid in the digestive process or to favorably influence food digestion and the immune system. The additives are particularly useful for encouraging animals to produce large amounts of commercially valuable products, such as liquid milk or meat. The increasing emphasis on reducing or eliminating the use of subtherapeutic antibiotics in animal feed in favor of natural alternatives, such as phytonutrients, has spurred research to explore which phytonutrients can be added to compositions used in encapsulation processes.

[0037]

[54] In these studies, plant extracts were increased as a source of phytonutrients in compositions used in drip granulation processes. The formulations contained 50% Lys HCl and 0.5% SMS emulsifier. To determine the integrity of the granulations, the prototype materials were placed in porous dacron bags and incubated in the rumen of lactating dairy cows for 16 hours.

[0038]

[55] The inclusion of plant extracts in the suspension reduced the ruminal integrity of the granules, with a more pronounced impairment of protein (lysine) integrity compared to dry matter integrity. These studies demonstrated that the incorporation of plant botanical or essential oil extracts into the slurry suspension required tailoring the viscosity and rheological properties of the matrix to optimally protect lysine. Due to the differential impact of essential oil solubility in the triglyceride matrix, more optimized emulsifier type and amount could result in a much more stable encapsulated product with higher protein recovery. For combined products, preferred compositions can be formulated to achieve a consistent release of phytonutrients and some lysine in the rumen, followed by complete dissolution in the gastrointestinal tract, thereby providing multiple benefits depending on the target biological activity of the phytonutrients and the associated benefits of soluble protein (lysine) proving resistant to the rumen or lower gastrointestinal tract. The results are shown in Table 3.

[0039] [Table 3]

[0040] Example 4. Effect of emulsifiers (polyglycerols, also called PGEs, are unique) on the rheological properties of lysine-lipid compositions

[56] Emulsifiers are widespread amphiphilic molecules used in a wide range of applications, including the food, feed, personal care and cosmetics, and pharmaceutical industries. Emulsifiers are highly versatile and can be used to achieve different functions, such as wetting agents, emollients, solubilizers, dispersants, antifoaming agents, crystal modifiers, and texturants. In addition, emulsifiers can also modify the fat nucleation, crystal growth, and polymorphic transformation processes not only in the bulk but also in the emulsion phase. This unique functionality offers a major breakthrough in the food industry, allowing customization not only to reduce saturated fatty acids in fatty acids but also to improve shelf life and sensory properties.

[0041]

[57] Generally, most emulsifiers contribute to the regulation of fat crystals in some way based on the size and type of head group, fatty acid chain, fat solubility, etc., but emulsifiers can be classified as crystal formers or crystal breakers. The solubility of emulsifiers, based on the similarities and differences of the fatty acid chains of the molecules, the emulsifier concentration, etc., contributes to various functions in the fat system. When a hydrophobic fat contains a large amount of hydrophilic water-soluble solid components such as sugars, the emulsifier should function to lubricate the solids and form a much less viscous slurry / suspension. In embodiments of the present disclosure, suitable emulsifiers can be identified based on the properties of the fat and dry solids, their particle size, and stability.

[0042]

[58] In one aspect of the present disclosure, processing steps for encapsulating lysine were investigated using hydrogenated soybean oil blended with the water-soluble solid Lys HCl. The amount of solid lysine, the lipid to lysine ratio, and the concentration and type of emulsifier were shown to affect the rheological properties of the blends processed to form granules or extruded products.

[0043]

[59] Furthermore, a differentiating feature of emulsifiers is their release characteristics of lysine after processing, which was important to understand whether emulsifiers affect the release of encapsulated hydrophilic ingredients.

[0044]

[60] To address these questions, 45:55 blends with hydrogenated soybean oil (Dritex S from Stratas Food, LLC) were prepared by melting the lipid in the presence of a 1% (w / w) concentration of emulsifier and gradually adding Lys HCl while stirring. Rheological measurements were performed using an AR-2000 Stress Controlled Rheometer from TA Instruments in a concentric cylinder geometry at shear rates ranging from 0.029 to 100 rad / sec at 85 °C.

[0045]

[61] Figure 4 shows the viscosity curves at 85°C as a function of shear rate in the presence of emulsifiers GMS - glycerol monostearate; SMS - sorbitan monostearate; 3-1-S - triglycerol monostearate; and 10-1-S - decaglycerol monostearate. The lysine particle size was <40 mesh. The chemical formulas for sorbitan monostearate (SMS) and glycerol monostearate (GMS) are shown below. Those skilled in the art will recognize that triglycerol monostearate has three glycerol groups instead of the single glycerol group of glycerol and sorbitan monostearate shown below, and decaglycerol monostearate has ten glycerol groups. [ka]

[0046]

[62] Compared to processing with monostearates, glycerol head groups with sorbitan esters of stearic acid were shown to be more effective in reducing the viscosity of lipid-lysine blends. Similarly, decaglycerol esters of stearic acid were more effective than the corresponding triglycerol esters. The common function of the head groups comes from their bulkiness. Larger fatty acid chain head groups are more oriented toward the solid / liquid interface, promoting lubrication of solid particles and, consequently, fluidizing the slurry and reducing its viscosity characteristics. The size distribution of solid particles in the fatty continuous phase determines the rheological performance.

[0047]

[63] Figure 5 shows the effect of fatty acid tail groups of emulsifiers with similar head groups. Sorbitan monostearate (SMS), sorbitan monooleate (SMO), and sorbitan monolaurate (SML) all share a common sorbitan head group and vary in the length of the fatty acid chain in the hydrophobic portion. The lower viscosity of lysine-lipid slurries containing SMS compared to SML suggests that emulsifiers with fatty acid chains more similar to the lipid system perform better. For the same reason, SMO increases viscosity more than any other emulsifier with a similar sorbitan ring.

[0048]

[64] Soy lecithin is a phospholipid with two fatty acid chains and a larger polar phosphate ester head group, and has the formula: [ka]

[0049]

[65] As mentioned above, phosphatidylcholine is generally considered an advantageous component of lecithin because it is rich in choline, a component of the B vitamin complex that is involved in certain biological functions. Phosphatidylcholine has the following formula: [ka]

[0050]

[66] Lecithin is a well-known food emulsifier. For example, lecithin is commonly used in chocolate production to reduce the viscosity of solid sugars. However, lecithin is not sufficient to improve the yield properties. Polyglycerol polyricinoleate (PGPR) is a polyglycerol ester-based emulsifier used in combination with lecithin, resulting in a synergistic interaction that improves the viscosity and yield properties of chocolate.

[0051]

[67] Further aspects of the present disclosure are illustrated in Figures 6-16.

[0052]

[68] Figure 6 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (10-1-S -decaglycerol monostearate, Yelkin® SS lecithin from Archer Daniels Midland Company, or 6-2-S -hexaglycerol monostearate) for a composition comprising encapsulated lysine according to an embodiment of the present disclosure, the composition comprising a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier.

[0053]

[69] Figure 7 illustrates the viscosity curve at 85°C as a function of shear rate in the presence of an emulsifier (Yelkin® SS lecithin or 10-1-S -decaglycerol monostearate from Archer Daniels Midland Company) for a composition comprising encapsulated lysine according to an embodiment of the present disclosure, the composition comprising a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and lysine HCl sieved through a 40 mesh sieve.

[0054]

[70] Figure 8 illustrates the viscosity curve at 85°C as a function of shear rate in the presence of an emulsifier (Yelkin® SS lecithin or 10-1-S -decaglycerol monostearate from Archer Daniels Midland Company) for a composition comprising encapsulated lysine according to an embodiment of the present disclosure, the composition comprising a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and lysine HCl sieved through a 60 mesh sieve.

[0055]

[71] The viscosity data of lecithin was compared with that of the polyglycerol ester emulsifier 6-2-S (hexaglycerol distearate) in lysine-lipid slurry blends. Both lecithin and 6-2-S have two fatty acid chains and head groups (phosphate ester vs. hexaglycerol), and their functions are very similar, with similar diglyceride effects. Comparing the two polyglycerols (PGE) 6-2-S and 10-1-S, the larger decaglycerol head group dominates the viscosity-reducing function. Those skilled in the art will recognize that the teachings of the present disclosure will allow for a wide variety of improvements in maximizing the dry solid loading of a given matrix system by using emulsifiers with a good balance of hydrophilic and hydrophobic moiety sizes and types.

[0056]

[72] Those skilled in the art will recognize that the features of the present disclosure can be modified based on process needs to achieve a tailored solution using a lipid system with a given dry solids loading / particle size distribution.

[0057]

[73] The effect of lecithin (e.g., Yelkin® SS lecithin) and sorbitan monostearate (SMS) at a concentration of 1% on the rheological parameters of slurries containing hydrogenated soybean oil (Dritex S) and lysine HCl (60 mesh and 100 mesh) in ratios of 50:50 and 45:55 is illustrated in Figures 9-12.

[0058]

[74] Figure 9 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (Yelkin® SS lecithin from Archer Daniels Midland Company) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 60 mesh sieve.

[0059]

[75] Figure 10 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (Yelkin® SS lecithin from Archer Daniels Midland Company) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 100 mesh sieve.

[0060]

[76] Figure 11 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (SMS - sorbitan monostearate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 60 mesh sieve.

[0061]

[77] Figure 12 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (SMS - sorbitan monostearate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 100 mesh sieve.

[0062]

[78] In the course of understanding the rheological parameters of the encapsulation process disclosed herein, slurries of hydrogenated soybean oil and lysine HCl were prepared in different ratios of 50:50, 45:55, and 40:60, with lysine HCl at 40 mesh, and the effect of two different emulsifiers, lecithin (Yelkin® SS lecithin) and decaglycerol monostearate (10-1-S), was compared as shown in Figures 13-14.

[0063]

[79] Figure 13 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (lecithin) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend, a 45:55 blend, or a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 40 mesh sieve.

[0064]

[80] Figure 14 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (10-1-S -decaglycerol monostearate) for compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 50:50 blend, a 45:55 blend, or a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and the lysine HCl was sieved through a 40 mesh sieve.

[0065]

[81] When blends of Dritex S-lysine were made with 50:50 and 45:55 ratios and different particle sizes of lysine, the absolute viscosities varied greatly, even based on the choice of emulsifier. The viscosity profile with lecithin was fairly independent of lecithin particle size, being only about 30 Pa.s at most. On the other hand, the viscosity with sorbitan monostearate was relatively high, about 120 Pa.s at low shear.

[0066]

[82] The Dritex S blend with 40 mesh lysine in the presence of PGE10-1-S was significantly lower than with lecithin. The effectiveness of the emulsifiers can be ranked as 10-1-S > lecithin > SMS. Those skilled in the art will recognize that, according to the teachings of the present disclosure, the overall performance will be based on the selection of dry solids particle size, target loading, fat system, ratios thereof, and type of emulsifier.

[0067]

[83] Figure 15 illustrates the viscosity curves at 85°C as a function of shear rate for compositions comprising encapsulated lysine in the presence of an emulsifier (Yelkin® SS Lecithin or Yelkin® SS Lecithin with phytonutrient essential oil, i.e., thymol, or mint oil, or curcumin from Archer Daniels Midland Company) according to embodiments of the present disclosure, where the compositions comprise either a 49:50 blend of hydrogenated soybean oil and lysine with 1% emulsifier and 1% wt:wt of phytonutrient essential oil, and the lysine HCl was sieved through a 40 mesh sieve.

[0068]

[84] Figure 16 illustrates the viscosity curves at 85°C as a function of shear rate in the presence of an emulsifier (SMS - sorbitan monostearate or phytonutrient essential oil, i.e., SMS - sorbitan monostearate in combination with thymol or peppermint oil or curcumin) of compositions comprising encapsulated lysine according to embodiments of the present disclosure, where the compositions comprise either a 49:50 blend of hydrogenated soybean oil and lysine with 1% emulsifier and 1% wt:wt of phytonutrient essential oil, and the lysine HCl was sieved through a 40 mesh sieve.

[0069]

[85] Addition of phytonutrient essential oils at low concentrations (1% wt:wt) to Dritex S-lysine (40 mesh) in a 49:50 ratio along with 1% Yelkin SS (lecithin) resulted in a significant change in viscosity profile. Given the teachings of this disclosure, one skilled in the art will recognize that the choice of essential oil will uniquely affect rheological properties and that the disclosed characteristics can be adjusted to fine-tune the composition and to benefit material handling and subsequent encapsulation processes.

[0070]

[86] Sorbitan monostearate (SMS) is more effective when using curcumin and thymol as phytonutrients, while lecithin is more effective when using peppermint oil as a phytonutrient. In accordance with the teachings of the present disclosure, those skilled in the art will recognize that the type of emulsifier can play a major role in adjusting the properties of a given composition in the process to obtain a more tailored solution.

[0071]

[87] The research disclosed herein demonstrates that the rheology of lysine-lipid systems is influenced by the particle size of the dry solids, the target loading, the lipid system, its ratio, and the type of emulsifier. By adjusting the particle size and emulsifier (or emulsifier combination), such as PGEs 6-2-S and 10-1-, it is possible to maximize the dry solids loading, perhaps 60-65% (e.g., for lysine) or 65-70% (for histidine), or to use a broader particle size distribution than would otherwise be used, specifically to tailor the rheology and obtain the desired final granule size. The particle size of amino acids such as lysine affects the dispersion of liquid triglyceride coatings. When the solids are very fine, the liquid system must overcome the particle-particle interactions of the fine solids to achieve good flow and coating properties. A larger particle size distribution allows for a more uniform coating of the fat system. However, very fine particle sizes increase the likelihood of larger aggregates forming, which retard the flow of the fat-lysine slurry. The packing density of larger particle size solids allows for the liquid triglyceride containing emulsifier to penetrate the packed system more uniformly than would be expected with very fine solids. The required content and choice of emulsifier system will vary when interacting with the properties of the botanical components. Those skilled in the art will recognize that, following this disclosure, they can precisely formulate compositions that are convenient for processing for manufacturing while also providing benefits to animals.

[0072] Example 5. Production of lysine granules by drop granulation processing

[89] To investigate the composition and production by drop granulation when continuous operation is performed, lysine granules were produced in a pilot-scale facility substantially similar to that shown in Figures 1-3.

[0073]

[90] To facilitate evaluation of the particle size of solids at 40–60% Lys HCl loadings, Lys HCl was sieved using a Rotex separator equipped with 40, 60, or 100 mesh sieves. Monoglyceride (Alphadim 90 SBK), sorbitan monostearate (SMS), lecithin emulsifier, or a combination was tested at 1% loading. The integrity of the prototype materials was evaluated by incubating them in the rumen of lactating dairy cows in porous Dacron bags for 16 hours. It was found that smaller granules were more easily produced by using finer lysine particles (<60 mesh), because larger particles (<40 mesh) would separate due to density differences between the solid lysine particles and the lipids if the slurry feed line was not agitated before the granulator. In addition, larger particles (<40 mesh) would likely clog the seal bar / nozzle on the granulator during start-up and shutdown, thereby preventing continuous processing. Lecithin appeared to decrease ruminal integrity; however, it was observed that agitating the slurry prior to drop granulation can trap air in the suspension, which can destabilize the granulation and cause loss of granulation integrity. Entrapped air in the granulation can create a relatively porous material that can act as capillaries when exposed to an aqueous environment such as the rumen. The results are shown in Table 4.

[0074] [Table 4]

[0075] Example 6. Effect of drip-granulated granules on ruminal stability

[92] Lysine granulation was prepared substantially as shown in Figures 1-3. The composition included 1% lecithin, 49% hydrogenated soybean oil, and 50% Lys HCl.

[0076]

[93] Lys HCl was milled and sieved in a rotex separator fitted with 60 or 100 mesh sieves to facilitate assessment of the particle size of the solid. The drop-granulated granules were collected from batches of approximately 45 kg in size, and the particle size distribution was assessed by sieving the resulting granules through a vibrating separator (Sweco) fitted with six sieves.

[0077]

[94] Healthiness was determined by incubating drop-granulated granules in porous dacron bags in the rumen of lactating dairy cows for 16 hours. In vitro testing involved exposing the remaining material after ruminal incubation to a buffered solution of enzymes that simulated intestinal fluids. Results from the in vitro testing are reported as estimated intestinal release rates. The estimated amount of metabolizable Lys (MP Lys) per 100 g of drop-granulated granules was calculated using the formula: MP Lys (g) / 100 g of product = Lys (%) x Stability (%) x Release Rate. The results are shown in Table 5.

[0078] [Table 5]

[0079]

[96] The percent lysine protection in the rumen (stability) was not significantly affected by the mesh size of Lys in the drop-granulated granules or the estimated granule size. However, the estimated percent intestinal release was superior with finer mesh Lys, as 100-mesh Lys had an average intestinal release of 84%, while 60-mesh Lys had an average release of 52%. This result suggests that when Lys in the 100-mesh formulation was present, MP Lys was superior to 60-mesh Lys (24.6 g vs. 14.4 g, respectively). A further finding was that when using the preferred Lys mesh size, 100-mesh Lys, smaller granule diameters (2.4–2.8 mm; 2.8–3.4 mm) were superior to larger granule diameters (3.4–4.0 mm). Smaller granules (2.4-3.4 mm) had better MP Lys than larger granules (3.4-4.0 mm), as smaller granules had better intestinal release rates (%).

[0080] Example 7. Processing Method for Producing Drop-Granulated Lysine

[98] Lysine granulation was manufactured substantially as shown in Figures 1-3. Multiple batches of approximately 45 kg were prepared, each with the same composition. The composition contained 1% lecithin, 49% hydrogenated soybean oil, and 50% Lys HCl. The Lys used in the composition was milled through a 100-mesh screen, and laser diffraction was used to determine the size grade (μM) of the milled Lys. 90% of the milled Lysine was <125 μM, with a median size of approximately 50 μM. Each 45 kg batch of drop-granulated granules was maintained as a separate lot. The lots were sieved using a Sweco equipped with six screens to determine particle size distribution. Based on the sieving, the lots were further divided into granules in the 2.4-2.8 mm and 2.8-3.4 mm ranges. Specific divided lots were selected for measurement with a hand-held micrometer to assess granulation particle size (n=15 samples per selected lot).

[0081]

[99] Additionally, the drop-granulated granules were imaged to determine the size of the lysine granules found in the drop-granulated granules. Randomly selected granules from each divided lot were cut with the cut surface facing up on a carbon spot. Samples were imaged using a scanning electron microscope operating at a numerical aperture of 1, a working distance of 10 mm, 15 kV, and 50x magnification using the backscatter component.

[0082]

[0100] The drop-granulated granules were subjected to ruminal stability testing and in vitro simulated intestinal release testing, and the MP Lys content of the lots was calculated as described in Example 6. The results are shown in Table 6.

[0083] [Table 6]

[0084]

[0102] Granules with diameters ranging from 2.8 to 3.4 mm or 2.4 to 2.8 mm had similar ruminal stability (70% vs. 69%), intestinal release (89% vs. 93%), and estimated MP Lys (24.4% vs. 25.2% g / 100 g). Thus, uniform drop-granulated granules with consistent stability and lysine release were produced.

[0085] Example 8. Lysine status of dairy cows administered drip-granulated granules

[0104] A study was conducted to determine the ability of drip granulated granules to improve lysine status in lactating dairy cows. Drip granulated granules were manufactured as described herein. Dairy cows were fed a diet formulated to provide sufficient nutrition to maintain body weight while also supporting high milk production.

[0086]

[0105] For each study, eight Holstein dairy cows [BW (mean ± SD) = 598.2 ± 64.1 kg; DIM = 117 ± 16] were assigned to one of four treatments in a 4 × 4 Latin square replicate design over a 7-day experimental period. The total duration of the two prototype experiments was 28 days. The 7-day period (d) was divided into a washout period (d1, no treatment delivered), three adaptation periods (d2-4) in which treatments were delivered in gelatin capsules, and a statistical estimation period (d5-7) in which treatments were also delivered in gelatin capsules. Treatments were as follows: cows were fed the basal diet plus 115 g of corn meal (CON); the basal diet plus 115 g of a commercial rumen-protected lysine source (AJP) (positive control); the basal diet plus 115 g of one example of the rumen-protected lysine source; and the basal diet plus 115 g of a second example of the rumen-protected lysine source throughout the study. This study was repeated four times to evaluate eight different examples, identified as A through H.

[0087]

[0106] Treatments were delivered twice daily (12-hour intervals) via 28 mL gelatin capsules (Structure Probe Inc., West Chester, PA) and administered orally using a doser. All cows received the same diet once daily at 13:00 h throughout the study. Drop-granulated granules were manufactured according to the present disclosure and contained 50-55% lysine HCl and 1% selected emulsifier. Ajipro-L (Ajinomoto Heartland Inc., 8430 W. Bryn Mawr, #650, Chicago, IL) was used as the AJP treatment.

[0088]

[0107] Complete ration (TMR) samples were obtained weekly, dried in a forced-air oven at 110°C for 24 hours, and analyzed for dry matter (DM). See AOAC Official Methods of Analysis, 16th Edition (AOAC, 1995a, Association of Official Analytical Chemists). Diet composition was adjusted weekly to accommodate changes in DM content. TMR intake and remaining amounts were recorded to determine each cow's intake based on weekly DM analysis. Complete ration samples were collected weekly (twice during the period) and stored at -20°C until analysis. Samples were pooled (n = 2) throughout the experiment and analyzed for DM, crude protein (CP), acid detergent fiber (ADF), neutral detergent fiber (NDF), lignin, nonfibrous carbohydrates (NFC), sugars, starch, fat, ash, total digestible nutrients (TDN), Ca, P, Mg, K, Na, Fe, Zn, Cu, Mn, Mo, S, and Se content using wet chemistry methods (Cumberland and Valley Analytical Services, Hagerstown, MD). TDN values ​​and net energy for lactation (NEL) were obtained from the laboratory and calculated based on the Nutrient Requirements of Dairy Cattle (NRC) (http: / / www.nap.edu / catalog / nrs / (2001)). Physical characterization of the TMR was performed weekly using a Penn State Particle Separator (Kononoff et al., 2003).

[0089]

[0108] Milking occurred three times daily at 04:30, 12:30, and 19:30. Milk yield was recorded at each milking, and samples were taken at each milking on days 5–7 of each period. A preservative (800 Broad Spectrum Microtabs II; D&F Control Systems, Inc., San Ramon, CA) was added to the samples, which were then stored in a refrigerator at 0°C for 3 days. The samples were then composited proportionally to the milk yield and sent to a commercial laboratory (Dairy One, Ithaca, NY) for analysis of fat, net protein, casein, milk urea nitrogen (MUN), lactose, and total solids content, as well as somatic cell count (SCC) using mid-infrared techniques (AOAC, 1995b).

[0090]

[0109] Blood samples were collected from the tail vein or artery of each cow (BD Vacutainer; BD and Co., Franklin Lakes, NJ) at 0800, 1000, 1200, and 1400 h on days 5, 6, and 7 of each period, and on days -3, -2, and -1 of the first period for use as covariates. Serum and plasma samples were collected by centrifugation of the tubes at 2,500 × g for 15 min at 4°C and stored at -80°C for further analysis. Plasma samples were pooled for each cow and collection day, and the amino acid profile was analyzed.

[0091]

[0110] The bioavailable lysine content of Examples A-H was determined by assessing the relative change in plasma free amino acid concentration when dairy cows were fed CON or administered AJP or the test product. This method assumes a positive linear relationship between absorbed lysine concentration and plasma lysine concentration. Numerous publications have demonstrated that this method is biologically valid and useful for determining the amount of absorbable lysine delivered to the abomasum or intestine of animals (Guinard and Rulquin, 1994; King et al., 1991; Rulquin and Kowalczk, 2003).

[0092]

[0111] The bioavailable lysine content of the encapsulated lysine products was determined by assessing plasma free lysine as a percentage of total amino acids (TAA) following a bolus administration of the test product or AJP to dairy cows. Commercially available AJP products have a reported bioavailable lysine content of 25.6 g per 100 g. Using this value, the following formula was used to estimate the bioavailable lysine delivery of test products A-H: grams of bioavailable lysine (grams per 100 g) = [(product plasma lysine (% relative to TAA) - control plasma lysine (% relative to TAA)) / (AJP plasma lysine (% relative to TAA) - control plasma lysine (% relative to TAA)] × 25.6.

[0093]

[0112] Table 7 shows the effect of AJP or Examples A-H administered to dairy cows on plasma free amino acid concentrations. Examples A and F did not induce a beneficial effect on plasma lysine content. Example A did not perform because the median granule size was outside the specified range, while F did not perform because the emulsifier (SMS) may have caused reduced lysine release in the abomasum and small intestine. Examples B, C, D, E, G, and H demonstrated various possibilities for delivering bioavailable lysine. Example C demonstrated excellent performance, delivering an estimated 36 g of bioavailable lysine per 100 g of product. This study demonstrated the benefits of improving lysine status in lactating dairy cows by encapsulating lysine using the processing methods disclosed herein.

[0094] [Table 7]

[0095] [Table 8]

[0096] [Table 9]

[0097] Example 9. Effect of encapsulated Lys on milk production in lactating dairy cows

[0115] A study was conducted to investigate the ability of drip-granulated granules to affect lysine status and milk production in lactating dairy cows. Drip-granulated granules were formed substantially as described herein. Lactating Holstein dairy cows were fed a diet formulated to provide nutrients sufficient for weight maintenance while supporting increased milk production. Eight Holstein dairy cows [BW (mean ± SD) = 598.2 ± 64.1 kg; DIM = 117 ± 16 kg] were assigned to one of four treatments in a 4 × 4 Latin square replicate design over a 7-day experimental period. The total duration of the two prototype experiments was 28 days. The 7-day period was divided into a washout phase (d1, no treatment delivered), three adaptation periods (d2-4) in which the treatment was delivered via gelatin capsules, and a statistical estimation period (d5-7) in which the treatment was also delivered via gelatin capsules. Treatments were as follows: cows were fed the basal diet plus 115 g corn meal (CON); the basal diet plus 115 g of a commercial rumen-protected lysine source (AJP) (positive control); the basal diet plus 115 g of drip-granulated Lys granules (identified as rumen-protected Lys A (RPL A)); and the basal diet plus 115 g of a second rumen-protected lysine prototype (identified as rumen-protected Lys B (RPL B)) for the study period.

[0098]

[0116] Milking occurred three times daily at 04:30, 12:30, and 19:30. Milk yield was recorded at each milking, and samples were collected at each milking on days 5–7 of each period. A preservative (800 Broad Spectrum Microtabs II; D&F Control Systems, Inc., San Ramon, CA) was added to the samples, which were then stored in a refrigerator at 0°C for 3 d. The samples were then combined proportionally to the milk yield and sent to a commercial laboratory for analysis of fat, net protein, casein, milk urea nitrogen (MUN), lactose, and total solids content, as well as somatic cell count (SCC) using mid-infrared techniques (AOAC, 1995b).

[0099]

[0117] The results are shown in Table 8. No treatment differences were observed for feed intake, body weight (BW), feed intake as a percentage of BW, milk production, or milk composition. Dry matter intake was higher in RPL B cows compared with AJP cows (P = 0.006). Milk production tended to be higher in RPL B cows compared with AJP cows (P = 0.07). Fat-corrected milk (3.5%) also tended to be higher in RPL B cows compared with AJP cows (P = 0.11). Protein percentage was higher in RPL B cows compared with AJP cows (P = 0.02; CONT3). Milk urea nitrogen concentration was lower in RPL B-treated cows compared with AJP-treated cows (P = 0.05); CON cows also had lower milk urea nitrogen concentration than AJP cows (P = 0.01). Somatic cell count was lower in RPL B cows compared with AJP cows (P = 0.005).

[0100] [Table 10]

[0101]

[0119] Differences were observed between RPL B and CON, with RPL B tending to have higher feed intakes and higher milk production. RPL B cows also had lower milk urea nitrogen concentrations compared to AJP cows, suggesting the latter may be more susceptible to protein degradation. These results suggest that the encapsulated Lys described herein can be used to improve intake and milk production in lactating ruminants compared to commercially available encapsulated Lys.

[0102] Example 10. Effect of emulsifiers on nutrient content and ruminal stability of granules

[0121] A series of tests were conducted to evaluate the relationship between emulsifier or surfactant selection and the ability to form granules with increased solid nutrient content. Lysine HCl was initially evaluated at particle sizes passing through a 60-mesh or 100-mesh sieve. Monoglyceride (Alphadim 90 SBK), sorbitan monostearate (SMS), lecithin emulsifier, or a combination was tested at 1% or 1.5% (as the solids content approached the viscosity limit for granule formation). Histidine, methionine, and choline chloride were then compared as alternative examples of the process to provide an initial estimate of loading and stability.

[0103]

[0122] Figure 18 shows the relationship between emulsifier composition, lysine HCl dosage, and rumen stability for 3-5 mm diameter granules. While SBK provided good rumen stability, viscosity limited the lysine content to approximately 55% of the composition. In contrast, the use of lecithin allowed for solids up to 65%. When SMS was used alone, solids reached an intermediate level of 60%, while rumen stability remained maintained, with protein values ​​(RUP, %CP) exceeding 70%. Increasing the solid dosage generally resulted in a curvilinear decrease in rumen stability. Combining SMS and lecithin improved rumen stability compared to lecithin and allowed for increased dosage rates compared to SMS.

[0104]

[0123] Comparing small or large granules containing 55% lysine HCl showed less difference in ruminal stability when SMS was used alone compared to the greater variability seen in compositions based on a 50:50 blend of yelkin and SMS, as shown in Table 9. Rumen stability could also be manipulated by increasing the amount of surfactant to alter viscosity, but in this case, increasing SMS from 1 to 1.5% of the composition decreased the stability of the small granules from 87.7% to 73.7% RUP (% CP).

[0105]

[0124] As shown in the table, the characteristics of the nutrients also influence the achievable loading rate and the stability of the resulting particles. Using emulsifier blends, it was possible to successfully form granules with solids contents of 60% for methionine, 65% for lysine HCl, and 70% for histidine. Choline HCl was also shown to demonstrate the potential for physical delivery of nutrients other than amino acids.

[0106] [Table 11]

[0107]

[0126] The results of this example demonstrate the possibility of tailoring the type and amount of emulsifier in the formation of encapsulated granules to accommodate multiple nutrients and tailor their delivery within the animal's gastrointestinal tract. For a given nutrient, amino acid, vitamin, or phytonutrient, the optimization of the material for proper nutrient delivery will develop based on the viscosity that allows granule formation, which is created by the physical properties of the solids and the composition of the emulsifier, and which also interacts with the solid loading rate, emulsifier content, and granule size.

[0108]

[0127] Aspects of the present disclosure include:

[0128] Selection of one or a combination of emulsifiers has been found to maximize the dry solids content in the slurry while fine-tuning the formulation based on characteristics such as amino acid hydrophilicity, particle size, and the inclusion of additional nutritional additives such as plant extracts. In one embodiment of the present disclosure, solids contents of greater than 50% are now possible in a drop granulation-landing process. A further novel and beneficial utility is the option to formulate compositions with maximum dry solids content, perhaps 60-65% (e.g., in the case of lysine HCl) or 65-70% (in the case of histidine), or to use particles with a wider distribution than would otherwise be possible, particularly when adjusting the rheology and final size of the desired granules. These concentrations exceed those of existing commercial products, thereby improving practical utility.

[0109]

[0129] The use of polyglycerol emulsifiers in animal encapsulation provides improved properties, at least compared to sorbitan esters. They also appear to be effective alternatives to lecithin. The use of emulsifiers such as PGE allows for increased solids content and / or greater flexibility in solid particle size.

[0110]

[0130] To improve animal utilization, functional additives such as enzymes or phytonutrients are included in the encapsulated amino acid product. Substances such as mint (menthol) and capsaicin can cause inflammation and alter blood flow in animals. By using phytonutrients that improve the absorption capacity of intestinal tissue, it can be assumed that the absorption and utilization of amino acids delivered to the intestine of ruminants using the encapsulated amino acid product produced according to the present invention will be higher than when using non-encapsulated, i.e., free, amino acid products.

[0111]

[0131] The inclusion of botanical ingredients further tunes the rheology based on its function within the material matrix, resulting in both increased and decreased viscosity for solids. For example, the inclusion of curcumin, through its interaction with lecithin, significantly increased viscosity compared to SMS. This suggests that a significant amount of fine-tuning and tailoring may be required to optimize a product's nutritional and functional delivery in a single product form.

[0112]

[0132] While the present invention has been particularly shown and described with reference to preferred embodiments thereof, those skilled in the art will recognize that various changes in form and details thereof can be made therein without departing from the scope of the invention as encompassed by the appended claims.

Claims

1. 1. A process for encapsulating amino acid particles, comprising: (a) mixing a monoglyceride with a hydrogenated vegetable oil, thereby forming a coating mixture; (b) mixing the coating mixture with amino acid particles to form a slurry; (c) forming a molten product by heating the slurry; (d) dripping the molten product onto a belt cooler as substantially uniform drop-granulated granules; A process involving:

2. 2. The process of claim 1, wherein the amino acid particles are selected from the group consisting of lysine particles, methionine particles, histidine particles, choline particles, and combinations thereof.

3. 10. The process of claim 1, wherein the molten product is conveyed to a granulator and drips from the granulator onto the belt cooler.

4. 4. The process of claim 3, wherein the molten product is filtered to remove undesirable large particles from the molten product before being conveyed to the granulator.

5. 4. The process of claim 3, wherein the granulator is configured to produce drop granulated granules having a diameter in the range of 1 to 25 mm.

6. 4. The process of claim 3, wherein the drip granulated granules comprise greater than 50% by weight of nutritional amino acids.

7. 4. The process of claim 3, wherein the drip granulated granules, when fed to a ruminant, deliver a large amount of absorbable amino acids for direct nutrition to the animal, wherein the amino acids are not substantially fermented in the animal's rumen.

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