阅读说明：本技术 生产用于反刍动物的囊化氨基酸的方法 (Method for producing encapsulated amino acids for ruminants ) 是由 希琳·S·巴赛斯 M·J·塞卡瓦 P·H·多恩 董硕佳 迈克尔·普莱斯 布拉德·罗曼 伊 于 2018-10-25 设计创作，主要内容包括：提供了一种对氨基酸颗粒进行囊化或包衣的方法,用以生产用于反刍动物的囊化氨基酸饲料产品。所述囊化氨基酸饲料产品包含基本均一的、圆形的和无尘的锭剂颗粒。当将所述囊化氨基酸饲料产品饲喂给反刍动物时,所述产品将大量可吸收的氨基酸递送给所述动物以进行直接营养供给,其中所述氨基酸基本不在所述动物的瘤胃中发酵。在一个方面,所述方法是低成本、高容量、连续的方法,其产生包含按重量计大于50％的营养氨基酸的组合物。所述锭剂颗粒的优异使用性能允许将其用以进一步配制为需要使营养素均匀分布在整个最终饲料混合物中的动物饲料。(A method of encapsulating or coating amino acid granules is provided for producing an encapsulated amino acid feed product for ruminants. The encapsulated amino acid feed product comprises substantially uniform, rounded and dust-free lozenge particles. When the encapsulated amino acid feed product is fed to a ruminant, the product delivers a large amount of absorbable amino acids to the animal for direct nutritional provision, wherein the amino acids are not substantially fermented in the rumen of the animal. In one aspect, the process is a low cost, high volume, continuous process that produces a composition comprising greater than 50% by weight of nutritive amino acids. The excellent use properties of the lozenge particles allow them to be further formulated into animal feeds requiring uniform distribution of nutrients throughout the final feed mixture.)

1. A method of encapsulating or coating an animal feed ingredient, the method comprising:

(a) mixing an emulsifier with a coating agent, thereby forming a coating mixture; and

(b) the coating mixture is placed on particles of an animal feed ingredient to encapsulate or coat the animal feed ingredient.

2. The method of claim 1, wherein the emulsifier is selected from the group of: lecithin, monoglycerides, sorbitan esters, polyglycerols and combinations thereof.

3. The method of claim 1, wherein the coating agent is selected from the group consisting of oils and fatty acids, and combinations thereof.

4. The method of claim 1, wherein the animal feed ingredient is an amino acid.

5. A method of encapsulating amino acid particles, the method comprising:

(a) mixing a monoglyceride with a hydrogenated vegetable oil, thereby producing a coating mixture; and

(b) mixing the coating mixture with amino acid particles to form a slurry;

(c) heating the slurry to form a product melt; and

(d) the product melt was deposited onto the belt cooler as substantially uniform and dust-free lozenge particles.

6. The method of claim 5, wherein the amino acid particles are selected from the group consisting of lysine particles, methionine particles, histidine particles, choline particles, and combinations thereof.

7. The method of claim 5, wherein the product melt is transported to a pastillator and deposited from the pastillator onto the belt cooler.

8. The method of claim 7, wherein the product melt is filtered to remove unwanted large particles from the product melt prior to conveying it to the pastillator.

9. The method of claim 7, wherein the pastillation machine is configured for producing pastille particles in the range of 1 to 25mm in diameter.

10. The process of claim 7, wherein lozenge particles produced comprise greater than 50% by weight of nutritive amino acids.

11. The method of claim 7, wherein when the produced lozenge granule is fed to a ruminant animal, a large amount of absorbable amino acids is delivered to the ruminant animal for direct nutritional provision, wherein the amino acids are not substantially fermented in the animal's rumen.

12. The method of claim 7, wherein said pastillation machine comprises a heated cylindrical stator, wherein said heated cylindrical stator comprises a perforated rotating housing that rotates concentrically about said stator and deposits said pastille particles across the working width of said belt cooler.

13. A substantially uniform and dust-free lozenge particulate product that when fed to a ruminant delivers to the animal a large amount of assimilable amino acids for direct nutritional provision, wherein the amino acids are not substantially fermented in the rumen of the animal.

14. A substantially uniform and dust-free lozenge granulated product according to claim 13 comprising greater than 50% by weight of nutritive amino acids.

15. A product produced by the method of any one of claims 1-12.

16. A pastillation particle comprising:

an amino acid;

an emulsifier; and

a coating agent;

wherein the shape of the pastillated particles is approximately hemispherical with an aspect ratio (diameter/height) of 1.5 to 2.5.

17. The pastillated particle as claimed in claim 16, wherein said amino acid is selected from the group consisting of lysine, histidine, methionine, choline and any combination thereof.

18. The pastillated particle as claimed in claim 16 or claim 17, wherein said emulsifier is selected from the group consisting of lecithin, monoglycerides, sorbitan esters, polyglycerol and combinations thereof.

19. The pastillated granule of any one of claims 16-18, wherein the coating agent is selected from the group consisting of oils, fatty acids, and combinations thereof.

20. The pastillated granule of any one of claims 16-18, wherein the coating agent is a hydrogenated vegetable oil.

21. The pastillated granule as claimed in any one of claims 16-20, wherein the size of the pastillated granule is from 2.2 to 5.0 mm.

22. The pastillated granule as claimed in any one of claims 16-20, wherein the size of the pastillated granule is from 2.2 to 3.5 mm.

23. The pastillated granule as claimed in any one of claims 16 to 22, wherein the amino acid has a particle size of 50-120 mesh.

24. The pastillated granule as claimed in any one of claims 16 to 22, wherein the amino acid has a particle size of 80-110 mesh.

25. The pastillated granule as claimed in any one of claims 16-22, wherein said amino acid is present in said pastillated granule in the range of 25% -85% by weight, 25% -75% by weight or 35% -75% by weight.

26. A method of feeding an animal, the method comprising:

mixing pastillated granules as claimed in any one of claims 16 to 25 with animal feed ingredients to produce an animal feed; and

feeding the animal with the animal feed.

27. The method of claim 26, wherein the animal is a ruminant.

28. A method of encapsulating amino acid particles, the method comprising:

mixing an emulsifier with a coating agent, thereby producing a coating mixture; and

mixing the coating mixture with amino acid particles to form a slurry;

forming pastilles from said slurry; and

depositing said pastilles on a belt.

29. The method of claim 28, further comprising heating the coating mixture.

30. The method of claim 28 or claim 29, further comprising cooling the pastilles on the belt.

Technical Field

The present invention relates to methods for preparing compositions for delivering large amounts of absorbable amino acids to ruminants for direct nutritional provision, and compositions prepared by the methods.

Background

Ruminants have evolved a large pre-gastric fermentation process that digests feed that is not normally digested by the mammalian hydrolytic enzymatic processes. A beneficial process associated with the fermentation of cellulose and other feeds is to provide the animal with nutritional end products such as microbial proteins, volatile fatty acids, and vitamins. However, high quality protein and free amino acids can ferment in the first stomach (also referred to as the "rumen") of ruminants, thereby reducing their values. In particular, if free amino acids are added directly to the diet, they are fermented to ammonia and volatile fatty acids, which are much less valuable to animals than amino acids. Rumen fermentation of feed (particularly amino acids) therefore presents a difficult challenge in formulating a diet that accurately supplies the essential amino acids required for ruminant animal maximum growth and lactation.

To achieve controlled amino acid delivery and release, various compositions and methods have been tested. Some of these methods have proven to be of practical and commercial value. However, it has proven difficult to develop and practice high capacity processing methods that consistently produce ruminal protective amino acids that are subsequently released in the small intestine. Conventional coating techniques and methods for making encapsulated products are expensive and can result in inconsistent product quality. Conventional coating materials typically have no functional purpose other than to protect amino acids from rumen microbial fermentation. Certain coatings, while protective, are not approved as safe in animal feed applications.

Various conventional protective barriers have been utilized. An effective barrier system limits the exposure of amino acids in feed through the rumen while readily releasing nutrients after exposure to the digestive processes of the acid enzyme compartment of the digestive tract. Commercial interest has focused primarily on predicting the amino acids with the greatest limitations on performance, such as methionine and lysine. Since each amino acid has unique chemical and physical characteristics, the barrier technology must be coordinated with one or more specific characteristics of the amino acid. Inclusion of amino acids in a protective matrix or shell adds expense and inevitably dilutes the amino acids provided by the feed product. Conventional methods have not met with adequate amino acid density in feed products, technical delivery, and cost-effective manufacturing techniques.

Disclosure of Invention

In one aspect of the present disclosure, a method of manufacture is provided that overcomes the limitations of conventional manufacturing techniques and surprisingly results in compositions that, when fed to ruminants, deliver large amounts of absorbable amino acids to the animal for direct nutritional provision. In one aspect, the method includes a deposition or pastillation technique that produces a composition comprising greater than 50% by weight of a nutritive amino acid. The process produces uniform sized particles (i.e., capsules or tablets) in a low cost, high volume, continuous process.

In one aspect, the method comprises encapsulating or coating an animal feed ingredient, the method comprising mixing an emulsifier with a coating agent to form a coating mixture, and placing the coating mixture on an animal feed ingredient pellet, thereby encapsulating or coating the animal feed ingredient.

In one aspect of the disclosure, a method mixes an emulsifier with a hydrogenated vegetable oil and heats, thereby producing a coating mixture, and mixes the coating mixture with amino acid particles to form a slurry. The method may further include heating the slurry to form a product melt. The method may further comprise depositing onto the belt cooler the product melted into substantially uniform and dust-free pastille particles by the pastillator.

Drawings

A more complete understanding of the present invention and the advantages thereof may be acquired by referring to the following description in consideration of the accompanying drawings, in which like reference numbers indicate like features, and wherein:

fig. 1 illustrates a flow diagram of a method in accordance with aspects of the present disclosure.

Figure 2 shows further aspects of the pastillation machine shown more generally in figure 1.

Figure 3 shows the placement of the product from the opening in the pastillator onto a cooling belt, which is shown more generally in figure 1.

Fig. 4 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of emulsifiers (GMS-glycerol monostearate, SMS-sorbitan monostearate, 3-1-S-triglyceride monostearate, and 10-1-S-decaglycerol monostearate) at 85 ℃, wherein the composition comprises a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, according to aspects of the present disclosure.

Figure 5 shows a viscosity curve as a function of shear rate for a composition comprising encapsulated lysine in the presence of emulsifiers (SMS-sorbitan monostearate, SM L-sorbitan monolaurate, and SMO-sorbitan monooleate) at 85 ℃ as a function of shear rate, wherein the composition comprises a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, according to aspects of the present disclosure.

FIG. 6 shows an emulsion (10-1-S-decaglycerol monostearate, Archer Daniels Midland Company) at 85 deg.CSS lecithin, or hexaglycerol 6-2-S-monostearate), a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine, wherein the composition comprises a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier.

FIG. 7 illustrates emulsifying agent (Archester Midland, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin or decaglycerol 10-1-S-monostearate), wherein the composition comprises a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 40 mesh screen.

FIG. 8 illustrates emulsifying agent (of Archer Dendrom, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin or decaglycerol 10-1-S-monostearate), a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine, wherein the composition comprises a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is passed through a 60 mesh screenAnd (4) screening.

FIG. 9 illustrates emulsifying agent (of Archer Dendrom, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin), wherein the composition comprises a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 60 mesh screen.

FIG. 10 illustrates emulsifying agent (of Archer Dendrom, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin), wherein the composition comprises a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 100 mesh screen.

Fig. 11 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (SMS-sorbitan monostearate) at 85 ℃, wherein the composition comprises a 50:50 blend of hydrogenated soybean oil and lysine or a 45:55 blend with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 60 mesh screen, according to aspects of the present disclosure.

Fig. 12 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (SMS-sorbitan monostearate) at 85 ℃, wherein the composition comprises a 50:50 blend of hydrogenated soybean oil and lysine or a 45:55 blend with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 100 mesh screen, according to aspects of the present disclosure.

Fig. 13 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (lecithin) at 85 ℃, wherein the composition comprises a 50:50 blend or 45:55 blend or 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 40 mesh screen, according to aspects of the present disclosure.

Fig. 14 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (10-1-S-decaglycerol monostearate) at 85 ℃, wherein the composition comprises a 50:50 blend or 45:55 blend or 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 40 mesh screen, according to aspects of the present disclosure.

FIG. 15 shows emulsifying agent (Archester Midland, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin orSs lecithin and phytonutrient essential oil, i.e. thymol or peppermint oil or curcumin), wherein the composition comprises a 49:50 blend of hydrogenated soybean oil and lysine with 1% emulsifier and 1% wt: wt phytonutrient essential oil, and wherein the lysine hydrochloride is screened through a 40 mesh screen.

Figure 16 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (SMS-sorbitan monostearate or SMS-sorbitan monostearate and a phytonutrient essential oil, i.e. thymol or peppermint oil or curcumin) at 85 ℃, wherein the composition comprises a 49:50 blend of hydrogenated soybean oil and lysine with 1% emulsifier and 1% wt: wt phytonutrient essential oil, and wherein lysine hydrochloride is screened through a 40 mesh screen, according to aspects of the present disclosure.

Figure 17 shows the effect of emulsifier/surfactant selection on lysine hydrochloride content and ruminal stability (RUP).

Detailed Description

Many conventional coating compositions incorporate lipids or fatty acids as hydrophobic and nutritionally acceptable materials to provide a basis for resistance to the rumen aqueous environment. The challenge is that the amino acids present in the formulation as dry solids have a different melting point and density than the lipids. Solubility differences based on the extreme hydrophilic and hydrophobic properties of amino acids and lipids generally result in phase separation of the slurry when mixed together in a molten state. Such phase separation can occur not only in the bulk phase, but also in the small molecules of the fat crystal network. The amino acids may be included in the formulation in the form of salts that incorporate the physical characteristics of particle distribution, or may be included in the aqueous solution in the form of "free" amino acids to enhance the considerations of hydrophobic and hydrophilic interactions. Separation of components within the matrix can lead to inconsistencies within the final product and reduce the level of protection against the rumen environment. In one aspect of the present disclosure, the amino acid may be an amino acid that is beneficial to the animal when added to the ruminant's diet, including but not limited to lysine, methionine, histidine, choline, and any combination thereof.

In one aspect of the present disclosure, new techniques are provided that overcome the challenges and limitations of conventional approaches. Experiments were designed and conducted that tested certain characteristics of solid particles, emulsifiers, lipids, and rheology of slurries prepared using the pastillation method. It has been surprisingly found that when rheological parameters are well controlled, a high percentage of solids can be incorporated into the slurry or product melt when the pastillation/deposition process is practiced.

In one aspect of the present disclosure, a slurry in a fluid state is provided for making uniform pastilles that meet target specifications. A more precise understanding of the rheology enables the selection of compositions comprising amino acids, lipids and emulsifiers (which can be adjusted for other additives, if desired).

The viscosity of the slurry increases with the solids content and the fineness of the incorporated solids (i.e., amino acids). The inclusion of an emulsifier helps to reduce the surface tension between the solid/liquid interface, which can lead to a reduction in viscosity. In addition, the shear thinning properties of the slurry allow for the inclusion of higher solids content, which makes the slurry flowable during processing. The similarity in fatty acid chain length and unsaturation between the emulsifier "tail" and the fat used may also improve function. It has been determined that, in general, for a given solids concentration and solids particle size, a larger "head" on the emulsifier can provide a greater reduction in viscosity. Common emulsifiers with good properties for animal food are sorbitan esters and lecithin (phosphatidylcholine is a component thereof). Phosphatidylcholine is generally considered a beneficial component of lecithin because it is rich in choline, a member of the B vitamin complex that is involved in certain biological functions. The presence of emulsifiers in systems with very high solubility parameters promotes the lubrication of solids in fatty systems by creating more nucleation sites. This allows for a higher loading of hydrophilic solids in the fat slurry, resulting in a more uniform dispersion and, in the process, a more uniform pastille.

Lecithin contains two fatty acid chains with a larger phosphate head group. Lecithin is described in the prior art in relation to compositions used in ruminant food and methods of producing encapsulated products, due to its advantageous emulsifying properties. Lecithin, although a food emulsifier is described in detail and is commonly used in chocolate manufacture to reduce the viscosity of sugar solids, is not suitable for improving the yield characteristics. Polyglycerol polyricinoleate (PGPR) is a polyglycerol ester based emulsifier, usually used in combination with lecithin to provide viscosity and yield properties, and due to synergistic interactions, combinations of lecithin-PGPR are common in chocolate manufacture. Surprisingly, it was found that a single emulsifier diglyceride showed comparable functionality to lecithin. Structurally similar emulsifiers, such as phospholipids and hexaglycerol distearate, exhibit similar functionality in controlling the rheological parameters of fat-lysine slurries. However, the larger polyglycerol (decaglycerol) is more effective than lecithin, enabling viscosity control in high solids slurries.

Fig. 1 illustrates a flow diagram of a method in accordance with aspects of the present disclosure. As shown in fig. 1, pastillation system 100 includes a mixing vessel 2, a pastillator 4, a belt cooler 6, and a bagging station 8. The raw material 10 and the coating mixture 12 may be added to the mixing container 2 through the upper opening 14 of the mixing container 2. The raw material 10 may comprise an amino acid supplied from an amino acid source 16. The coating mixture 12 may include an emulsifier and a coating agent, which are mixed and supplied from a coating mixture source 18. The mixing arm 20 may be rotated about a vertical axis a-a to mix the raw materials 10 and the coating mixture 12 within the mixing vessel 2 to form a slurry. The feedstock 10 and coating mixture 12 may be heated in the mixing vessel 2 to form a product melt 22. For example, the raw material and coating mixture may be heated to above 10 ℃ above the melting point of the fat. In alternative embodiments (not shown in fig. 1), the raw materials 10 and the coating mixture 12 may be heated together or separately prior to mixing in the mixing vessel 2, or together after mixing in the mixing vessel 2. Product melt 22 may exit mixing vessel 2 through a lower opening 24 of mixing vessel 2. The product melt 22 may be pumped from the mixing vessel 2 to the pastillator 4 using a pump 26. In one embodiment, product melt 22 may flow to filter 28 to remove unwanted large particles or agglomerates so that a substantially uniform filtered product melt may exit filter 28 and be conveyed or delivered to pastillator 4.

The pastillator 4 is configured to heat the filtered product melt to maintain the flowability of the product melt 22 and form pastilles comprising encapsulated amino acids. The pastillator 4 is configured for depositing substantially uniform and dust-free lozenge particles 30 (comprising 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 and dust-free lozenge particles 30 can be substantially hemispherical. In another embodiment, the substantially uniform and dust-free lozenge particles can have a substantially pyramidal shape (similar to the chocolate crumb shape). In one embodiment, the lozenge particles have an aspect ratio (diameter: height) of 1.5 to 2.5, about 1.7, or about 2.0, and are shaped like a hemisphere. In another embodiment, the substantially uniform and dust-free lozenge particles may be substantially flat-edged spheres (similar to the shape of an ice hockey puck). The pastiller 4 may be configured to produce pastille sizes of the desired size, for example in the range of 1 to 25mm in diameter (when looking down at the pastille particles after deposition on the belt cooler 6). Lozenge particles 30 may be collected from the distal end 34 of the belt cooler 6 and transported to the bagging station 8 where they may be placed in a bag 36. The pastillator 4 can be operated continuously for a long time. Water may be pumped from the water tank 40 by the cooling water pump 38 into the cooler 42 and then delivered to the cooling water sprayer 44 containing the spray nozzle 46. Cooling water may be sprayed by the spray 44 through the nozzles 46 to the bottom boundary surface 48 of the belt cooler 6 and thereby provide cooling to the belt cooler 6 and the lozenge particles 30 on the belt cooler 6. After spraying, the water may be circulated back to the water tank 40. The belt cooler 6 may rotate about belt rollers 50 and 52. As shown in fig. 1, belt roller 50 is proximal to flyer 4 and belt roller 52 is distal to flyer 4.

The excellent use properties of the lozenge particles allow them to be further formulated into animal feeds requiring uniform distribution of nutrients throughout the final feed mixture.

Fig. 2 shows further aspects of the pastillation machine 4 shown more generally in fig. 1. As shown in fig. 2, the pastillator 4 includes a product distribution tube 200, a heat shield 204, a heated cylindrical stator 206, a heating medium 208, and a product distribution rod 210. The pastillator 4 may also include a re-feed bar 212. As previously described, the pastillator 4 is configured to deposit substantially uniform and dust-free pastille particles 30 (comprising encapsulated amino acids) onto the belt cooler 6. The filtered product melt supplied from filter 28 (shown in fig. 1) is heated by pastillator 4 to maintain the flow capacity of product melt 22. Product melt 22 is deposited on the belt cooler 6 through product dispensing port 202 as substantially uniform and dust-free lozenge particles 30 comprising encapsulated amino acids. The cooling water nozzles 46 are configured to spray cold water onto the interface 48 to cool the belt cooler 6 and the lozenge particles 30 deposited on the belt cooler 6. The belt cooler 6 may include belt rollers 216. Belt roller 216 may be the same as or different from belt rollers 50 and 52. The vertical distance between the belt cooler 6 and the pastillator 4 can be adjusted by moving the rollers 216 vertically relative to the pastillator 4.

The heated cylindrical stator 206 may include hollow rollers 218. Heated cylindrical stator 206 may include a perforated rotating housing 220 that rotates concentrically about the stator to deposit droplets of product melt 22 as pastille particles 30 across the working width of steel belt or belt cooler 6. The baffle and internal nozzle system built into the heated cylindrical stator 206 provides uniform pressure across the working width of the belt cooler 6, thereby providing uniform flow through all of the holes or product dispensing ports 202 of the perforated rotating housing 220. This ensures that along a row of lozenge particles 30 from one edge of the strip to the other, each lozenge particle 30 is of uniform size.

The peripheral speed of the pastillator 4 is synchronized with the speed of the belt so that the droplets are deposited on the belt without deformation. The heat released during the solidification and cooling process is transferred to the cooling water sprayed below through the stainless steel belt or belt cooler 6. This water is collected in a water tank, such as water tank 40, and returned to a water cooling system or chiller 42, and at no stage is the water in direct contact with the product or lozenge particles 30. The design of an effective pastillation system takes into account a number of factors. For example, the minimum diameter of the lozenge is dependent on the diameter of the hole or product dispensing opening 202 in the rotating housing 220, the density and viscosity of the product itself, surface tension, and mechanical acceleration applied to the drop. Those skilled in the art will recognize that in accordance with the present disclosure, the droplets should be of sufficient weight and volume to deposit on the steel belt or belt cooler 6, and the distance between the outer rotating housing 220 and the steel belt can be adjusted to provide an efficient process and the desired pastille particles 30.

Those skilled in the art will recognize that appropriate process parameters and component configurations may be further refined in light of this disclosure using specially developed computer programs and/or test runs using specific products to be processed.

Fig. 3 shows the deposition of lozenge particles 30 on the belt cooler 6. As shown in fig. 3, lozenge particles 30 are deposited on the belt cooler 6 through product dispensing opening 202. Those skilled in the art having the benefit of this disclosure will recognize that suitable pin and/or needle configurations may be used to transport lozenge particles 30 through the product dispensing opening 202 onto the belt cooler 6.

In one aspect, a product produced by any of the methods described herein is produced.

In another aspect, the pastillated granules comprise an amino acid, an emulsifier, and a coating agent. The shape of the pastillated granules is approximately hemispherical with an aspect ratio (diameter/height) of 1.5 to 2.5.

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 a combination thereof. The coating agent may be selected from the group consisting of oils, fatty acids, and combinations thereof. The coating agent may be a hydrogenated vegetable oil. The size of the pastillated granules may be 2.2-5.0mm or 2.2-3.5 mm. The amino acid may have a particle size of 50-120 mesh or 80-110 mesh. The amino acid may be present in the pastillated granules in a range of 25% to 85% by weight, 25% to 75% by weight, or 35% to 75% by weight.

In another aspect, a method of feeding an animal comprises mixing pastillated pellets produced as described herein with animal feed ingredients to produce an animal feed, and feeding the animal feed to the animal. The animal may be a ruminant.

In another aspect, a method of encapsulating amino acid particles includes mixing an emulsifier with a coating agent to produce a coating mixture, mixing the coating mixture with amino acid particles to form a slurry, forming lozenges with the slurry, and depositing the lozenges onto a belt. The method may further comprise heating the coating mixture and/or cooling the pastilles on the band.

Other aspects of the methods and encapsulated products of the present disclosure are further described in connection with the following examples.

Example 1. effect of lysine particle size and emulsifier use on rumen integrity (viscosity as a distinguishing characteristic).

The following examples demonstrate viscosity as a distinguishing characteristic according to aspects of the present disclosure. A test was conducted to evaluate the equipment and granulation process during spray cooling. The objective of these tests was to form pellets of about 1mm and to evaluate the effect of lysine content and particle size and emulsifier selection on rumen integrity (stability). Lysine hydrochloride in dry powder form was added at 50% to the slurry. The lysine hydrochloride is ground and supplied with a larger particle size distribution or screened through a 40 mesh screen. Hydrogenated soybean or palm oil makes up the balance of the formulation. During the test, 25 pound batches of slurry were formed using a rotating disk running in a spray tower. The results are shown in table 1.

In this experiment, the yield of acceptable particle size was low and rumen stability was poor compared to commercial encapsulated products. The slurry mixes poorly and the slurry is "tough", especially for a broader spectrum of coarser materials (i.e., <40 mesh lysine particles). When the solids are greater than 50% and separation of the slurry is observed, viscosity and flowability become problems. The slurry requires a high loading of emulsifier to show a suitable flow rate for spray cooling with 50% solids. High emulsifier content may be detrimental to encapsulation. Hydration of the particles results in stable dispersion in an aqueous environment. However, the method of accomplishing encapsulation is also an important parameter in the formation of rumen-stable products.

Example 2 evaluation of lysine formulation in processing (viscosity affects processing method-therefore control can be made to improve product).

A series of studies were conducted to evaluate the processing regime (granulation, fluid bed coating, extrusion and pastillation) and the interaction of the composition with the process lysine hydrochloride with different particle size profiles (L ys HC L) (unscreened L ys HCl and screened L ys HCl) was used in the formulation the slurries were formulated to contain 40% or 50% L ys HCl and 0.5% to 5% monoglyceride emulsifier by weight of the formulation ((R) ()) was added90SBK, supplied by Colebeon (Corbion) and higher than the said fatThe fat system is heated to about 20 degrees celsius of its melting point. The remainder of the material was fully hydrogenated soybean oil. The coating process utilized fully hydrogenated soybean oil plus emulsifier sprayed on lysine particles. After incubation in the rumen of lactating cows for 16 hours, the rumen stability of the samples of each prototype was evaluated. The results are shown in table 2.

The prototype resulting from spray cooling makes the pellets more spherical because the viscosity increases as the particle size becomes somewhat larger. Reducing lysine content improves rumen stability. Extrusion provides flexibility for formulation of lysine suspensions and formation of granules, however, disruption along the granule edges appears to compromise rumen integrity. Fluid bed processing results in rumen integrity superior to spray cooling and is similar to extrusion.

Pastillation processing may result in pellets with superior integrity, particularly when the particle size of L ys HCl is controlled at <40 mesh it has been found that viscosity can be adjusted sufficiently to enable pastillation of high solids suspensions with pastilles having an average particle size greater than 2 mm.

Example 3. functional additives included in the composition further differentiate and aid in nutritional supply.

Animals present various challenges in commercial feeding operations that can compromise health care or reduce nutritional supply due to malabsorption or altered gastrointestinal tract function. Feed additives, in particular naturally occurring phytonutrients found in plant extracts (botanic and dplant extracts), are often added to feed to support the digestion process or to favorably influence the digestion of the feed and the immune system of the animal. The additives are particularly useful for animals producing large quantities of products of commercial value, such as liquid milk or meat. Increasing emphasis is being placed on reducing or eliminating the use of subtherapeutic antibiotics in animal feed, supporting natural alternatives (e.g. phytonutrients), prompting research to explore whether phytonutrients can be added to compositions used in the encapsulation process.

In these studies, plant extracts as a source of plant nutrients increased the composition used during pastillation the formulation contained 50% L ys HCl and 0.5% SMS emulsifier the prototype material was incubated in a porous dacron pouch in the rumen of a lactating cow for 16 hours to assess the integrity of the pastilles.

The inclusion of plant extracts in the suspension reduced the rumen integrity of the troches, significantly compromising the integrity of the protein (lysine), compared to the dry weight integrity. These studies indicate that the incorporation of botanical or essential oil extracts into slurry suspensions requires adjustment of the viscosity and rheological properties of the matrix to provide optimal protection of lysine. Because of the different solubility effects of essential oils in triglyceride bases, more desirable emulsifier types and amounts can provide a more stable encapsulated product with higher protein recovery. In a combination product, preferred compositions can be formulated to release an amount of phytonutrients and some lysine in the rumen and then undergo absolute dissolution in the gastrointestinal tract, thereby providing multiple benefits depending on the targeted biological activity of the phytonutrients and the benefits associated with providing soluble protein (lysine) to the rumen or lower digestive tract. The results are shown in table 3.

TABLE 3

Example 4. effect of emulsifiers on the rheological properties of lysine-lipid compositions (polyglycerol, also known as PGE, is unique).

Emulsifiers are ubiquitous amphiphilic molecules and are found in a wide range of applications in the food, feed, personal care and cosmetic and pharmaceutical industries. Emulsifiers are used in a wide variety of applications and are therefore developed for different functions, such as wetting agents, emollients, solubilizers, dispersants, antifoams, crystal modifiers, texturizers, etc. In addition, the emulsifier may also alter the nucleation, crystal growth and polymorphic transformation processes of fat not only in the bulk phase but also in the emulsified phase. This unique functionality provides a major breakthrough for the food industry in that the customized fat system not only reduces saturated fat, but also improves shelf life and organoleptic properties.

While most emulsifiers typically promote modification of the fat crystals in some form based on the size and type of head group, fatty acid chains, solubility in fat, etc., emulsifiers may be classified as either crystal formers or crystal breakers. Different functionalities are contributed to the fat system based on similarities and dissimilarities in the fatty acid chains of the molecules, solubility of the emulsifiers, concentration of the emulsifiers, etc. When the hydrophobic fat has a high amount of hydrophilic water-soluble solid components, such as sugars and the like, the functionality of the emulsifier should be such that it lubricates the solids, thereby forming a much lower viscosity slurry/suspension. In aspects of the present disclosure, suitable emulsifiers may be identified based on the nature of the fat as well as the dry solids, their particle size and stability.

The amount of lysine solids, the ratio of lipid to lysine, and the concentration and type of emulsifier were shown to affect the rheology of the blends processed to form pastilles or extruded products.

In addition, the distinguishing feature of emulsifiers is the release profile of lysine after processing. It is important to know whether emulsifiers will affect the release of the encapsulated hydrophilic ingredients.

To solve these problems, a 45:55 blend of hydrogenated soybean oil (Dritex S from stelatas Food, LL C) was made by melting the lipids at a concentration of 1% (w/w) in the presence of an emulsifier and gradually adding L ys HCl with stirring rheological measurements were made using an AR-2000 stress controlled rheometer from TA Instruments (TA Instruments) with concentric cylinder geometries having shear rates in the range of 0.029 to 100 rad/sec at 85 ℃.

FIG. 4 shows GMS-glyceryl monostearate as an emulsifier at 85 ℃; SMS-sorbitan monostearate; viscosity curves as a function of shear rate in the presence of triglyceride 3-1-S-monostearate and decaglycerol 10-1-S-monostearate. The particle size of lysine was <40 mesh. Sorbitan Monostearate (SMS) and Glycerol Monostearate (GMS) have the following chemical formulas. Those skilled in the art will recognize that tristearin will have three glycerin groups, while decaglyceryl monostearate will have ten glycerin groups, rather than the single glycerin groups shown below for glyceryl monostearate and sorbitan monostearate.

Sorbitan monostearate

Glyceryl monostearate

The glycerol head group of sorbitan stearate was shown to be more effective in reducing the viscosity of lipid-lysine blends than the monostearate being treated. Similarly, decaglycerol stearate is more effective than the corresponding triglyceride. The general functionality of the head group comes from its body. The larger the head group, the more the fatty acid chains are oriented towards the solid/liquid interface and help lubricate the solid particles, thereby fluidizing the slurry, resulting in low viscosity characteristics. The rheological functionality is driven by the particle size distribution of the solid particles in the fat continuous phase.

Sorbitan Monostearate (SMS), Sorbitan Monooleate (SMO) and sorbitan monolaurate (SM L) all have a common sorbitan ester head group, while the fatty acid chain length of the hydrophobic portion varies the viscosity of SMS-containing lysine-lipid slurries is lower compared to SM L, indicating that the emulsifier is relatively more functional when the fatty acid chain is more similar to the lipid system.

Soybean lecithin is a phospholipid having two fatty acid chains and a larger polar phosphate head group, and is represented by the following formula:

polyglycerol fatty acid ester

n is the number of glycerol units

As mentioned previously, phosphatidylcholine is generally considered a beneficial component of lecithin because it is rich in choline, a member of the B vitamin complex that is involved in certain biological functions. The following formula shows phosphatidylcholine:

phosphatidylcholine

Lecithin is a well-known food emulsifier. For example, lecithin is commonly used in chocolate manufacturing to reduce the viscosity of sugar solids. However, lecithin does not improve the yield properties well. Polyglycerol polyricinoleate (PGPR) is a polyglycerol ester based emulsifier used in combination with lecithin to provide the viscosity and yield characteristics of chocolate and its synergistic interaction.

Aspects of the present disclosure are further illustrated in fig. 6-16.

FIG. 6 shows emulsifying agent (10-1-S-decaglycerol monostearate, Archer Dennieri Midland, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin, or hexaglycerol 6-2-S-monostearate), a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine, wherein the composition comprises a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier.

FIG. 7 illustrates emulsifying agent (Archester Midland, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin or decaglycerol 10-1-S-monostearate), wherein the composition comprises a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 40 mesh screen.

FIG. 8 illustrates emulsifying agent (of Archer Dendrom, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin or decaglycerol 10-1-S-monostearate), wherein the composition comprises a 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 60 mesh screen.

In the case of the lysine-lipid slurry blend, the viscosity data for lecithin was compared to the polyglycerol ester emulsifier 6-2-S (hexaglycerol distearate). Both lecithin and 6-2-S have two fatty acid chains and a head group (phosphoric acid vs hexaglycerol) and are very similar in functionality, showing similar diglyceride effects. When comparing two polyglyceryl esters (PGE)6-2-S and 10-1-S, the larger decaglycerol head group dominates the viscosity reducing functionality. In light of the teachings of the present disclosure, one skilled in the art will recognize that the use of emulsifiers having a good balance of sizes and types of hydrophilic and hydrophobic moieties can provide a wide variety of improvements in maximizing dry solids loading in a given matrix system.

One skilled in the art will recognize that the features of the present disclosure can be modified based on process needs to achieve a customized solution for a given loading/particle size distribution of dry solids in a lipid system.

FIGS. 9-12 show lecithin at 1% (e.g., concentration)SS lecithin) and Sorbitan Monostearate (SMS) in the rheological parameters of slurries of hydrogenated soybean oil (Dritex S) and lysine hydrochloride (60 mesh and 100 mesh) at 50:50 and 45:55 ratios.

FIG. 9 illustrates emulsifying agent (of Archer Dendrom, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin), wherein the composition comprises a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 60 mesh screen.

FIG. 10 illustrates emulsifying agent (of Archer Dendrom, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin), wherein the composition comprises a 50:50 blend or a 45:55 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 100 mesh screen.

Fig. 11 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (SMS-sorbitan monostearate) at 85 ℃, wherein the composition comprises a 50:50 blend of hydrogenated soybean oil and lysine or a 45:55 blend with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 60 mesh screen, according to aspects of the present disclosure.

Fig. 12 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (SMS-sorbitan monostearate) at 85 ℃, wherein the composition comprises a 50:50 blend of hydrogenated soybean oil and lysine or a 45:55 blend with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 100 mesh screen, according to aspects of the present disclosure.

In understanding the rheological parameters of the encapsulation process disclosed herein, hydrogenated soybean oil and lysine hydrochloride slurries were prepared with different ratios of 50:50, 45:55 and 40:60 of 40 mesh lysine hydrochloride and two different emulsifiers lecithin (as shown in figures 13-14) were comparedSS lecithin) and decaglycerol monostearate (10-1-S).

Fig. 13 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (lecithin) at 85 ℃, wherein the composition comprises a 50:50 blend or 45:55 blend or 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 40 mesh screen, according to aspects of the present disclosure.

Fig. 14 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (10-1-S-decaglycerol monostearate) at 85 ℃, wherein the composition comprises a 50:50 blend or 45:55 blend or 40:60 blend of hydrogenated soybean oil and lysine with 1% emulsifier, and wherein the lysine hydrochloride is screened through a 40 mesh screen, according to aspects of the present disclosure.

When Dritex S-lysine blends were prepared with lysine having different particle sizes at ratios of 50:50 and 45:55, their absolute viscosities varied greatly even based on the choice of emulsifier. The viscosity curve of lecithin is completely independent of the particle size of lecithin, the higher viscosity range being only 30 pa.s. However, the sorbitan monostearate has a relatively high viscosity at low shear in the range of 120 pa.s.

The blend of Dritex S with lysine of 40 mesh in the presence of PGE 10-1-S was much lower than lecithin. The effectiveness of the emulsifiers may be ranked as 10-1-S > lecithin > SMS. In light of the teachings of the present disclosure, one skilled in the art will recognize that overall functionality will be based on the selection of particle size of the dry solids, target loading, fat system, their ratios, and emulsifier type.

FIG. 15 shows emulsifying agent (Archester Midland, Inc.) at 85 deg.C, according to aspects of the present disclosureSS lecithin orSS lecithin and phytonutrient essential oil, i.e. thymol or peppermint oil or curcumin), wherein the composition comprises a 49:50 blend of hydrogenated soybean oil and lysine with 1% emulsifier and 1% wt: wt phytonutrient essential oil, and wherein the lysine hydrochloride is screened through a 40 mesh screen.

Figure 16 shows a viscosity profile as a function of shear rate for a composition comprising encapsulated lysine in the presence of an emulsifier (SMS-sorbitan monostearate or SMS-sorbitan monostearate and a phytonutrient essential oil, i.e. thymol or peppermint oil or curcumin) at 85 ℃, wherein the composition comprises a 49:50 blend of hydrogenated soybean oil and lysine with 1% emulsifier and 1% wt: wt phytonutrient essential oil, and wherein lysine hydrochloride is screened through a 40 mesh screen, according to aspects of the present disclosure.

When a low concentration (1% wt: wt) of plant nutrient essential oil was added to Dritex S-lysine (40 mesh) containing 1% Yelkin SS (lecithin) at a ratio of 49:50, a significant change in the viscosity curve was observed. In light of the teachings of the present disclosure, one skilled in the art will recognize that rheological properties are solely influenced by the choice of essential oil, and that the properties of the present disclosure can be tailored to fine tune the composition and benefit material transport and subsequent encapsulation processes.

Sorbitan Monostearate (SMS) was more effective as a phytonutrient for curcumin and thymol, while lecithin was more effective as a phytonutrient for peppermint oil. In light of the teachings of the present disclosure, one skilled in the art will recognize that the type of emulsifier may play a major role in adjusting the properties of a given composition in a process for more tailored solutions.

The studies disclosed herein show 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. Adjusting the particle size and the emulsifier (or combination of emulsifiers), such as 6-2-S and 10-1-of PGE, can be done to the maximum extent of dry solids, perhaps 60% -65% (e.g., in the case of lysine) or 65% -70% (in the case of histidine), or alternating with a broader particle distribution profile than would otherwise be practical, especially depending on the rheology and desired final lozenge size. The particle size of the amino acid (e.g., lysine) affects the distribution of the liquid triglyceride coating. In the case of very fine solids, the liquid system must overcome the particle-particle interactions of the fine solids to provide good flow and coating characteristics. If the particle size distribution is larger, the coating of the fat system may be more uniform. However, as the particle size is finer, there is a greater likelihood of forming larger aggregates that can impede the flow characteristics of the fat lysine slurry. The bulk density of the larger particle size solids allows for more uniform penetration of the liquid triglyceride and emulsifier into the bulk system than would be desirable from very fine solids. Interaction with the characteristics of the plant components will then alter the desired levels and selection of the emulsifier system. One skilled in the art will recognize that, in light of the present disclosure, precise compositions can be formulated that facilitate manufacturing processes, while also providing utility in animals.

EXAMPLE 5 lysine pastilles made by pastillation processing

Lysine pastilles were produced in pilot scale equipment substantially as shown in figures 1 to 3 to investigate the composition and pastillation manufacture when practiced in a continuous operation.

The integrity of the prototype material was evaluated by incubating in a porous dacron bag in the rumen of lactating cows for 16 hours.it has been found that smaller diameter lozenges can be more easily manufactured using finer particle size lysine (<60 mesh) because the larger particles in <40 mesh result in separation of solids in the slurry feed line before the pastillator due to density differences between the solid lysine particles and the lipid.moreover, during start and stop periods in the process, the larger particles in <40 mesh block the sealing bar/nozzle on the pastillator.

Example 6 Effect of pastillated granules on rumen stability

Lysine pastilles were produced substantially as shown in figures 1 to 3 the composition comprised 1% lecithin, 49% hydrogenated soybean oil and 50% L ys HCl.

The L ys HCl was ground and sieved on a rotating sieve fitted with a 60 mesh or 100 mesh sieve to facilitate evaluation of the solid particle size the pastilled particles were collected from a batch of about 45kg and sieved through a vibratory separator (Sweco) fitted with 6 sieves to evaluate the particle size distribution of the pastilled particles formed.

The integrity of the lozenge granules was determined by incubation in a porous dacron bag in the rumen of lactating cows for 16 hours the material remaining after incubation in the rumen was exposed to an enzyme buffer solution mimicking intestinal fluid in an in vitro assay the results of the in vitro assay are reported as estimated intestinal release the estimated metabolizable L ys (MP L ys) amount per 100g of pastilled granules was calculated using the following formula: g MP lysine/100 g product ═ L ys x% stability x release the results are shown in table 5.

Table 5.

The% protection (stability) of lysine in the rumen is largely unaffected by the mesh size of L ys in pastillated granules or the assumed size of the granules, however, when a finer mesh L ys is used, the estimated% intestinal release rate is superior because the 100 mesh L ys average intestinal release rate is 84% and the 60 mesh L ys average intestinal release rate is 52%. the results show that 100 mesh vs 60 mesh L ys in the composition yields a superior MP L ys (24.6 vs 14.4g, respectively). further, it was found that within the preferred L ys mesh diameter of 100 mesh L ys, smaller diameter pastilles (2.4-2.8; 2.8-3.4mm) yield superior MP L ys. smaller pastilles (2.4 to 3.4mm) compared to larger diameter pastilles (3.4-4.0mm), 24.8-3.4 mm) yield better MP L ys. smaller pastilles (24.4 to 3.4mm) because of smaller MP L% release is better than larger diameter pastilles (3.4-4 mm).

Example 7. processing to produce spindle lysine.

Lysine pastilles are produced substantially as shown in figures 1 to 3. batches of about 45kg, each with the same composition, the composition comprises 1% lecithin, 49% hydrogenated soybean oil and 50% L ys hcl. L ys used in the composition is ground through a 100 mesh screen and laser diffraction is used to determine the size grade (μ M) of L ys after grinding, 90% of the milled lysine is less than 125 μ M, each batch of pastilled particles having a median size of about 50 μm.45kg remains as a unique batch.

The pastillated particles were further subjected to imaging techniques to determine the size of the lysine particles found in the pastillated particles. Randomly selected lozenges in each sub-batch were sliced and placed on carbon dots with the cut side up. The sample was imaged using a scanning electron microscope operating with backscatter compensation, aperture 1, 10mm working distance, 15kV and 50x magnification.

Rumen stability and in vitro simulated intestinal release assays were performed on the pastillated granules and the MP L ys content of the batches was calculated as described in example 6 the results are presented in table 6.

Table 6.

Lozenges with diameters of 2.8-3.4mm or 2.4-2.8mm had similar rumen stability% (70 vs 69), intestinal release% (89 vs 93) and estimated MP L ys (24.4 vs 25.2g/100 g).

Example 8 lysine status given to cows that were pastillated.

A study was conducted to determine the ability of the pastillated granules to improve the lysine status of lactating cows. The pastillated granules were produced as described herein. Cows are fed a diet formulated to provide nutrients sufficient to maintain body weight while supporting large milk production.

For each study, eight holstein cows BW (mean ± SD) 598.2 ± 64.1kg, DIM 117 ± 16] were assigned to 1 of 4 treatments in a repeated 4 × 4 latin square design with a length of 7 days, total length of experiment of 2 prototypes 28 days the experimental period (7 days (d)) was divided into an elution period (day 1, no treatment was delivered), an adaptation period 3 (days 2 to 4) in which treatment was delivered in gelatin capsules, and a statistical inference period (d days 5 to 7) in which treatment was also delivered in gelatin capsules treatment was as follows, basic diet +115g corn meal (CON), basic diet +115g rumen-protecting lysine source (AJP) (positive control), one example of basic diet +115g rumen-protecting lysine source, and a second example of basic diet +115g rumen-protecting lysine source, the entire study was continued.

Treatment was delivered twice daily by 28m L gelatin capsules (structural Probe Inc., west chester, pennsylvania) delivered twice daily (12 hours apart) and administered orally by a drug applicator (balling gun.) during the entire trial all cows were fed the same diet at 1300h each day.

Total Mixed Ration (TMR) samples were taken weekly and analyzed for Dry Matter (DM) by drying in a forced air oven for 24 hours (h) at 110 ℃, see AOAC official Analytical methods 16 th edition (AOAC, 1995a, official Analytical chemists' Association.) diet composition was adjusted weekly to change DM content of the composition TMR provided and refused for each cow was recorded to determine intake based on weekly DM analysis, lumped mixed ration samples were taken weekly (2 times per cycle) and stored at-20 ℃ until analysis, Wet chemical methods (Camberland Valley analysis service (Cumberland Valley Analytical Services), Black Grangston, Maryland) were used to analyze DM, Crude Protein (CP), Acid Detergent Fiber (ADF), Neutral Detergent Fiber (NDF), clean lignin, non-fibrous carbohydrate (NFC), sugar, starch, fat, ash, Total Digestible Nutrients (TDN), Ca, Na, Zn, Sep, Mn.

Cows were milked 3 times per day at 0430, 12300 and 1930 h. Milk weight was recorded at each expression and samples were taken at each expression on days 5 to 7 of each period. Preservatives (800Broad Spectrum Microtabs II; D & F control Systems, Inc., san lamon, california) were added to the samples and mixed in proportion to the milk production, stored in a refrigerator at 0 ℃ for 3 days and sent to a commercial laboratory (Dairy One, isa, n.y.) for analysis of fat, true protein, casein, Milk Urea Nitrogen (MUN), lactose, total solids content and Somatic Cell Count (SCC) using an infrared program (AOAC, 1995 b).

Blood samples were collected from the caudal vein or artery of each cow on days 0800h, 1000h, 1200h and 1400h of each period and used as covariates on days-3, -2 and-1 of the first period (BD Vacutainer; BD corporation, franklin lake, new jersey.) serum and plasma samples were obtained by centrifuging tubes at 2500 × g for 15 minutes at 4 ℃ and stored at-80 ℃ for further analysis.

Bioavailable lysine content of examples a-H was determined by assessing the relative change in plasma free amino acid concentration when feeding cows either CON or AJP or the test product. This method assumes that the absorbed lysine is in a positive linear relationship with plasma lysine concentration. A number of publications have demonstrated that this approach is biologically relevant and is useful in determining the delivery of absorbable lysines to the stomata or intestinal tract of animals (Guinard and Rulquin, 1994; King et al, 1991; Rulquin and Kowalczk, 2003).

The bioavailable lysine content of the encapsulated lysine product when the test product or AJP was injected into cows was determined by assessing the percentage of plasma free lysine content to Total Amino Acids (TAAs). The reported bioavailable lysine content of the commercially available AJP product was 25.6g/100 g. This value was used to estimate the delivery of bioavailable lysine for test products a to H using the following equation: the grams of lysine bioavailable (grams per 100g) — 25.6 [ (product plasma lysine,% of TAA-CONT plasma lysine%, TAA ]/(AJP plasma lysine,% of TAA-CONT plasma lysine%, of TAA) ].

Table 7 shows the effect of AJP or examples a to H administration to cows on plasma free amino concentration. Examples a and F did not elicit a beneficial effect on plasma lysine content. Example a failed because the troches were outside the specified range of the median troche size, while F failed because the emulsifier (SMS) may cause poor release of lysine in the abomasum-small intestine. Examples B, C, D, E, G and H demonstrate the different potential for bioavailable lysine delivery. Example C demonstrated superior properties and estimated delivery of 36g of bioavailable lysine per 100g of product. Studies have shown the benefit of improving the lysine status of lactating cows by encapsulating lysine using the processing methods disclosed herein.

TABLE 7 plasma free amino acid concentrations (. mu.M/L) and bioavailable lysine content of prototype encapsulated lysine products A-H

Example 9 influence of encapsulated lysine on milk production in lactating cows.

A study was conducted to study the ability of pastillated pellets to affect lysine status and milk yield of lactating cows spindle pellets formed substantially as described herein feeding lactating holstein cows a diet formulated to provide nutrition sufficient to maintain body weight while supporting a large amount of milk yield eight holstein cows BW (mean ± SD) 598.2 ± 64.1kg, DIM ═ 117 ± 16] to 1 of 4 treatments in a repeated 4 × latin square design, the length of the experimental period being 7 days, the total length of 2 prototypes being 28 days the experimental period (7 days) being divided into an elution period (day 1, no treatment delivered), an adaptive 3 period (days 2 to 4) in which treatment is delivered in the form of gelatin capsules, and a statistically inferred period (days 5 to 7) in which treatment is also delivered in the form of gelatin capsules feeding corn meal +115g (basal diet), CON +115g + commercially available dietary supplementation, a protected diet, (115 g + 29 g) and a protected rumen protected diet (a) as well as protected rumen protected diet supplemented by lysine, protected diet, protected by dietary supplementation, protected by cow rumen, protected by a diet, stabilized by a, stabilized by stabilized diet, stabilized by.

Cows were milked 3 times per day at 04:30, 12:30 and 19:30 hours. Milk weight was recorded at each expression and samples were taken at each expression on days 5 to 7 of each period. Preservatives (800Broad Spectrum Microtabs II; D & F control Systems, Inc., san lamon, california) were added to the samples and mixed in proportion to the milk production, stored in a refrigerator at 0 ℃ for 3 days and sent to a commercial laboratory for analysis of fat, real protein, casein, milk urea nitrogen, lactose, total solids content and Somatic Cell Count (SCC) using an infrared program (AOAC, 1995 b).

The results of the study are presented in table 8 feed intake, Body Weight (BW), feed intake as a percentage of BW, milk yield or milk composition without treatment differences RP L B cows have a higher dry matter intake (P0.006) compared to AJP, RP L B cows have a higher milk yield (3.5%) compared to AJP, RP L B cows have a higher protein percentage (P0.07) compared to AJP cows, RP L B cows have a higher fat-corrected milk (3.5%) compared to AJP, RP L B cows have a higher protein percentage (P0.02; CONT3) compared to AJP cows have a lower urea nitrogen concentration (P0.05) in cows given to RP L B compared to 637, and CON have a lower urea nitrogen concentration (P630.01) compared to AJP and lower body cells (P L B) compared to P6852.005).

Table 8.

A distinction is made between RP L B and CON, where RP L B shows a higher feed intake and a higher tendency towards milk production, furthermore, the cows of RP L B have a lower concentration of milk urea nitrogen than the cows of AJP, indicating that the latter may be more proteolytic than the latter, the results of this study demonstrate that encapsulation L ys formed by the method described herein can be used to improve feed intake and milk production in lactating ruminants compared to commercially available encapsulation L ys.

Example 10. effect of emulsifiers on lozenge nutritional composition and rumen stability.

A series of studies were conducted to evaluate the relationship of emulsifier or surfactant selection to the ability to form lozenges with increasing nutritional solids content. Lysine hydrochloride having a particle size passing through a 60 mesh or 100 mesh screen was first evaluated. Monoglyceride (Alphadim90SBK), Sorbitan Monostearate (SMS), lecithin emulsifier or combination were studied at 1% addition or 1.5% with solids content approaching the viscosity limit to form pastilles. Histidine, methionine and choline chloride were then compared as alternative examples of this method to form a preliminary estimate of loading rate and stability.

FIG. 18 shows the relationship between emulsifier composition, added lysine hydrochloride level and rumen stability of pastilles between 3-5mm in diameter. The use of SBK provided good rumen stability, but the viscosity limited the content of lysine to about 55% of the composition, compared to an increase in the solid content allowed to 65% on this test using lecithin. SMS alone is an intermediate to achieve a solids content of 60% while maintaining rumen stability greater than 70% (RUP, CP%) of the protein value. Increasing solid loading generally results in a decrease in the curve for rumen stability. The combination of SMS and lecithin provides improved rumen stability compared to lecithin and increased potential loading rates compared to SMS.

As presented in table 9, comparison of pastilles or pastilles containing 55% lysine hydrochloride showed less difference in rumen stability when SMS was used alone compared to the larger variance of the composition based on a 50:50Yelkin and SMS blend. Rumen stability can also be controlled by changing viscosity as surfactant levels increase, where pastille stability decreases from 87.7% to 73.7% RUP (% of CP) as SMS increases from 1% to 1.5% of the composition.

As presented in the table, the characteristics of the nutrients also affect the achievable loading rate and the stability of the resulting granules. The emulsifier blend was successfully formed into lozenges with a solids content of methionine of 60%, a solids content of lysine hydrochloride of 65% and a solids content of histidine of 70%. Choline hydrochloride has also been proposed to demonstrate the potential for physical delivery of nutrients other than amino acids.

Table 9.

The results of this example demonstrate the ability to adjust the type and level of emulsifier to accommodate multiple nutrients in the formation of encapsulated particles, as well as the potential to adjust delivery within the animal gut. The material optimization for a given nutrient, amino acid, vitamin or phytonutrient will develop from the viscosity developed by the physical characteristics of the solid and emulsifier composition such that particle formation also interacts with the solid loading rate, emulsifier content and particle size to provide proper delivery of the nutrient.

Aspects of the present disclosure include:

it was found that one or a combination of one or more emulsifiers were selected to maximize the dry solids content in the slurry and the formulation was fine-tuned for the addition of amino acid properties (e.g., hydrophilicity, particle size) and other nutritional additives (e.g., plant extracts). In one aspect of the present disclosure, a solids content of more than 50% during the ingot deposition process can be achieved. A further use which is of benefit to the novelty is the choice of formulating compositions which contain to the greatest extent dry solids, possibly up to 60% -65% (e.g. in the case of lysine hydrochloride) or 65% -70% (in the case of histidine), or alternatively using a broader particle distribution profile than would otherwise be practical, especially adjusted to the rheology and desired final lozenge size. These concentrations exceed those of the products commercially available on the market at present, which makes it possible to have improved practicality in practice.

The use of polyglycerol emulsifiers in capsules for animals, which provide improved properties over at least sorbitan esters, and they appear to be an effective substitute for lecithin. The use of emulsifiers such as PGE can allow for greater solids content and/or greater flexibility in solid particle size.

Functional additives, such as enzymes or plant nutrients, are included in encapsulated amino acid products to increase animal utilization. Mint (menthol) and capsaicin can alter inflammation or blood flow in animals. By using phytonutrients to enhance the absorptive capacity of intestinal tissues, it can be concluded that by using the encapsulated amino acid product prepared according to the present invention, the absorption and utilization of amino acids delivered to the ruminant intestine is higher compared to non-encapsulated amino acid products (i.e., free amino acid products).

The inclusion of botanical drugs, based on their function in the material matrix, brings additional adjustments to the rheology, both in viscosity increase and decrease relative to the solids observed. For example, curcumin, which contains interactions with lecithin, increases viscosity to a greater extent than is the case with SMS, suggesting that extensive fine tuning and customization may be required to optimize the product delivering nutrition and function in a single product form.

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