Micronized corn protein products and milk replacers containing same

Abstract

Micronized corn protein products may be used as a protein source in milk replacer formulations. The micronized corn protein product has a particle size distribution wherein d10 is from about 3 to about 9 microns, d50 is from about 8 to about 35 microns, d90 is from about 15 to about 70 microns, and d99 is from about 80 to about 95 microns. The micronized corn protein product has a protein content of at least about 50% dry weight; and a moisture content of less than about 14%.

Description

MICRONIZED CORN PROTEIN PRODUCTS AND MILK REPLACERSCONTAINING SAMECROSS-REFERENCE TO RELATED APPLICATIONS

[0001] This application claims the benefit of U.S. Provisional Patent Application No. 63 / 636,142, filed 19 April 2024, which is hereby incorporated by reference in its entirety.FIELD

[0002] The present invention relates to corn protein. More specifically, the present application relates to micronized corn protein products and milk replacers containing same.BACKGROUND

[0003] Milk replacers are commonly used for feeding young animals, and particularly calves, because they provide a low-cost alternative to providing nutrition as a substitute to the use of valuable cow’s milk. Because milk replacers are provided in powder form that is mixed with water just prior to use, they can be more easily stored than a perishable liquid. Typical milk replacers are formulated from components of milk, combined with an alternative protein source. Protein sources previously used include whey protein concentrate, dried skim milk, caseinates, dried whey, soy protein isolate, soy protein concentrate, and modified wheat protein. “See, Dairy Ingredients Used in Calf Milk Replacers - June 2016”, ADPI Intelligence Volume IV, Issue 1.

[0004] Compositions useful as a protein source for a milk replacer in animal feed are described in US 6,096,353 where a composition consists of a combination of hydrolyzed soya proteins and hydrolyzed cereal proteins is provided in a milk replacer formulation used for pre-ruminant and young ruminant calves, suckling piglets and suckling lambs. The use of cereal proteins selected from the group comprising wheat, barley, rye, oats, sorghum and corn is also described.

[0005] Similarly, milk replacer compositions comprising from 1-20 parts by weight of vegetable protein concentrate or isolate; and from 8-20 parts by weight of a carbohydrate source comprising 10-90% processed starch and 90-10% maltodextrin, together with whey powder and / or delactosed whey powder and / or whey protein concentrate, fat and additives are described in WO 2000 / 048474.SUMMARY

[0006] While animal milk replacer compositions are in principle a lower cost alternative to whole milk feeding, these compositions importantly should have chemical, physical and nutritional characteristics similar to milk and provide the young animals being fed (especially calves) with necessary nutrients for growth and rumen development. Typically, milk replacers are provided in powder form to be mixed on site at farms with water in a ratio of approximately 1 : 15. In order to be reliably prepared in conventional farm environments, all ingredients of the milk replacer (including added protein) need to be fully soluble / dispersible, without forming sediment under conditions of use. For that reason, ingredients that could easily sediment, such as corn gluten meal and other corn protein sources, are not used in animal milk replacer production.

[0007] Conventional corn protein sources, such as com gluten meal, are not particularly soluble in water under conditions of mixing that would be encountered in preparation of milk replacer compositions, and the protein of conventional corn gluten meal is likewise not fully digestible by young animals being fed with a liquid milk replacer composition that has had the conventional corn gluten meal mixed in without further formulation modifications.

[0008] It has been surprisingly been found that corn protein materials can be physically processed to be soluble / dispersible at concentrations suitable for incorporation in dry milk replacer formulations by providing the corn protein materials in the form of micronized corn protein product having a selected particle size distribution wherein dlO is from about 3 to about 9 microns, d50 is from about 8 to about 35 microns, d90 is from about 15 to about 70 microns, and d99 is from about 80 to about 95 microns.

[0009] In an aspect, the micronized corn protein product has a particle size distribution wherein dlO is from about 3 to about 10 microns, d50 is from about 8 to about 45 microns, and d90 is from about 15 to about 99 microns.

[0010] The micronized corn protein product has a protein content of at least about 50% dry weight, and a moisture content of less than about 12%. In an aspect, the micronized corn protein product has a protein content of from about 50% to about 98% dry weight.

[0011] The micronized com protein product having the characteristics as described herein are indicated to be surprisingly digestible by young animals, which is not the case for conventional corn protein products having larger average particle sizes. For example, it is indicated that conventional corn protein products having average particle greater than about 200 microns aretypically not digestible by young animals. Micronized corn protein products having the characteristics as described herein therefore advantageously provide excellent nutrition benefits when incorporated in a milk replacer formulation.

[0012] Moreover, the micronized corn protein products may exhibit good color in the dry and liquid form, and additionally have a flavor that is apparently well accepted by the animals to be fed without the need to incorporate additional flavorants or flavor masking materials.

[0013] It has been additionally found that micronized com protein products having the characteristics as described herein are surprisingly easy to mix with water under conventional conditions of use in preparing a liquid milk replacer composition, and so provide convenience to persons tasked with preparing liquid milk replacer compositions. The micronized corn protein products as described herein may exhibit low to no observed sedimentation under conventional conditions of use in preparing a liquid milk replacer composition. This performance characteristic provides a significant advantage, because sedimentation will lead to inhomogeneities when liquid is added to the dry composition to form the liquid milk replacer composition. Additionally, avoiding generation of an undue amount of sedimentation in the thus formed liquid milk replacer composition advantageously may reduce or eliminate plugging of orifices of dispensers (such as nipples used to feed young animals), thereby avoiding failure in being able to feed animals.

[0014] Dry micronized corn protein products as described herein are stable from a food safety perspective for storage for long periods of time when properly stored, and therefore very suitable for use as a component in a dry milk replacer composition designed to use in preparing a liquid milk replacer composition by addition of liquid (usually water).

[0015] Surprisingly, micronized corn protein products when mixed with liquid (such as water) for use in preparation of liquid milk replacer compositions are stable (i.e., experiences a low amount of sedimentation) for the time required to complete preparation of the liquid milk replacer compositions and administration of the liquid composition to the animals in need thereof.

[0016] The micronized com protein products having the characteristics as described herein therefore provide a naturally sourced protein product that can be used without inclusion of aids (“solvation additives”) to promote suspension of the micronized corn protein in water. Avoidance of such solvation additives advantageously provides a final milk replacer formulation with a “clean” ingredient declaration that is attractive to the consumer.

[0017] It has been found that the superior stability of the micronized corn gluten meal as compared to conventional com gluten meal, in combination with the superior digestibility of the micronizedcorn gluten meal as compared to conventional corn gluten meal provides unique and efficient addition of a naturally sourced com protein product in a final milk replacer formulation.BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate several aspects of the invention and together with a description of the embodiments serve to explain the principles of the invention.

[0019] A brief description of the drawings is as follows:

[0020] FIG. 1 is a graph showing the Stable Protein Solution Volume of various samples at pH 4.5.

[0021] FIG. 2 is a graph showing the Stable Protein Solution Volume of various samples at pH 6.2.

[0022] FIG. 3 is a graph showing body weight data for calves over the first 14 days in a study of various milk replacer formulations.

[0023] FIG. 4 is a graph showing milk replacer intake by calves over the first 14 days in a study of various milk replacer formulations.

[0024] FIG. 5 is a graph showing milk replacer concentrate intake by calves over the first 14 days in a study of various milk replacer formulations.

[0025] FIG. 6 is a graph showing CMR (calf milk replacer) drinking speed by calves over the first 14 days in a study of various milk replacer formulations (bars correspond to same samples as FIG. 5).DETAILED DESCRIPTION

[0026] The aspects of the present invention described below are not intended to be exhaustive or to limit the invention to the precise forms disclosed in the following detailed description. Rather a purpose of the aspects chosen and described is by way of illustration or example, so that the appreciation and understanding by others skilled in the art of the general principles and practices of the present invention can be facilitated.

[0027] For purposes of the present discussion, a corn protein starting materials and final micronized com protein products alike (jointly referred to as “com protein material(s)”) are considered to be “dry” if the material has a moisture content of less than about 14%. It has been found that corn protein materials having a moisture content of less than about 14% by weight tend to not have undesirable microbial growth during storage, and do not experience storage andhandling issues that arise from a change in flow properties due to excess moisture content. In an aspect, the corn protein material has a moisture content of less than about 12%. In an aspect, the corn protein material has a moisture content of less than about 10%. In an aspect, the corn protein material has a moisture content of less than about 8%. In an aspect, the corn protein material has a moisture content of less than about 6%. In an aspect, it is advantageous to not attempt to dry the corn protein material to an excessively low moisture content, since the cost of drying does not achieve a particular benefit when the com protein material is already sufficiently dry to achieve the above benefits. In an aspect, the moisture content of the corn protein material is not less than about 3.5%. In an aspect, the corn protein material has a moisture content of from about 3.5% to about 8%.

[0028] The corn protein starting material used for preparing the micronized com protein product may be any com protein material that provides the desired amount of protein content. Typically, the micronized com protein product has the same protein content as the corn protein starting material, i.e., the micronization process does not substantially reduce the protein content of the material being processed.

[0029] As noted above, the com protein starting material has a protein content of at least about 50% dry weight. In an aspect, the com protein starting material is a com gluten meal product, which comprises the com protein separated in, for example, a com wet-milling process, that additionally comprises quantities of starch and fibrous fractions not recovered separately from the protein in the primary separation process. Typical commercially available corn gluten meal products comprise from about 50% to about 65% dry weight protein. Corn gluten meal is commercially available from a number of sources, such as Cargill. An example of a commercially available corn gluten meal is Cargill 60% Com Gluten Meal, which is a high energy protein composition commonly provided at 60 percent dry weight protein.

[0030] It has been found that use of corn gluten meal products having a protein content of from 50% to about 65% dry weight as the corn protein starting material is advantageous because these starting materials are readily available and relatively inexpensive because production of this material does not include a substantial number of expensive processing steps.

[0031] In an aspect, the corn protein starting material is a corn protein concentrate or corn protein isolate. For purposes of the present discussion a protein concentrate is a protein composition having a protein content of from about 55% to about 85% dry weight, or having a protein content of from about 65% to about 85% dry weight. For purposes of the present discussion a proteinisolate is a protein composition having a protein content of from about 85% to about 100% (or 98%) dry weight.

[0032] It has been found that use of com protein sources having a protein content of from about 65% to about 85% dry weight, or from about 85% to about 100% dry weight, as the com protein starting material is advantageous because the resulting micronized corn protein product comprises fewer extraneous materials and provides a more concentrated delivery of protein in the ultimate dry milk replacer formulation as compared to conventional corn gluten meal.

[0033] The concentration of protein throughout this present disclosure is determined by nitrogen concentration using the Dumas protein analysis method as provided in accordance with AACC 46-30.01 (Crude Protein - Combustion Method) using a nitrogen analyzer (LECO TmSpecNTM, St. Joseph, Michigan USA) and a conversion factor of 6.25.

[0034] In an aspect, the corn protein concentrate is prepared as described in U.S. Patent No. 9,226,515 (assigned to Cargill Incorporated, and incorporated herein by reference). A typical analysis of such corn protein concentrate (e.g., Empyreal® 75, Cargill, Incorporated, Wayzata, MN) comprises about 75 wt% to 80 wt% protein on a dry weight basis, about 4.5% fat, about 5% soluble carbohydrates, and other nutrients (as-is basis), and has a bright yellow or gold color.

[0035] In an aspect, the com protein isolate is prepared by further treating a destarched corn protein material is then further treated in a solvent-mediated defatting step, by application of a water-miscible solvent / water defatting composition comprising from about 55% to about 90% water-miscible solvent to provide a com protein isolate. In an aspect, the water-miscible solvent is ethanol. In an aspect, the water-miscible solvent is isopropanol or other water-miscible solvent, and mixtures thereof.

[0036] In an aspect, the corn protein isolate has an L* color value of from about 88 to 95, an “a*” color value ranging from about -0.5 to 1.5, and a “b*” color value ranging from about 10 to 25; iii) has a soluble carbohydrate concentration of 40 g / kg or less; and iv) comprises at least about 85 wt % protein on a dry basis.

[0037] The micronized corn protein product is prepared by grinding the com gluten meal with equipment such as micronizers, pin mills, roller mills, hammer mills or impact mills. The fine particles thus produced may be subjected to a separation step according to size, weight, shape, density criteria or according to colorimetric characteristics, using equipment such as classifiers, screeners, separators, sieves, densimetric tables and combinations thereof.

[0038] In an aspect, the micronized corn protein product is prepared by micronization in a Hosokawa Milling Zirkoplex-classifier mill ZPS mechanical impact mill, optionally having anintegrated ALPINE ATP Turboplex Ultrafine Classifier. In an aspect, this system may be used in combination with a final sieve step to remove particles having a size above a desired upper limit and / or to achieve the desired particle size distribution.

[0039] Particle size distribution is determined by laser diffraction techniques using commercially available instrumentation, such as the Mastersizer 3000 from Malvern Instruments Limited.

[0040] For purposes of the present discussion, the particle size distribution is described in terms of percentile values, e.g. dlO, d50 and d90. These are statistical parameters that can be read directly from the cumulative particle size distribution. These percentile values indicate the size below which 10%, 50% or 90% of all particles are found.

[0041] As noted above, the micronized com protein product having a particle size distribution wherein dlO is from about 3 to about 9 microns d50 is from about 8 to about 35 microns d90 is from about 15 to about 70 microns, and d99 is from about 80 to about 95 microns.

[0042] In an aspect, the micronized corn protein product has a particle size distribution wherein dlO is from about 4 to about 8 microns d50 is from about 9 to about 30 microns d90 is from about 17 to about 65 microns, and d99 is from about 80 to about 95 microns.

[0043] In an aspect, the micronized corn protein product has a particle size distribution wherein dlO is from about 3 to about 10 microns, d50 is from about 8 to about 45 microns, and d90 is from about 15 to about 99 microns.

[0044] For purposes of the present discussion, D[4,3] is weighted mean value by volume. In other words, D[4,3] is center of mass for frequency distribution in units of volume.

[0045] In an aspect, the micronized corn protein product has a particle size distribution wherein D[4,3] is from about 8 to about 40. In an aspect, the micronized corn protein product has a particle size distribution wherein D[4,3] is from about 8 to about 50.

[0046] For purposes of the present discussion, D[3,2] is the surface moment mean diameter, i.e., the “Sauter mean.” In other words, D[3,2] is the diameter of a particle whose ratio of volume to surface area is the same as that of the complete sample. Mathematically, if V is the total volume and A is the total surface area of the sample, D3,2 = 6 * (V / A).

[0047] In an aspect, the micronized corn protein product has a particle size distribution wherein the micronized corn protein product has a particle size distribution wherein D[3,2] is from about 5 to about 20. In an aspect, the micronized corn protein product has a particle size distribution wherein the micronized corn protein product has a particle size distribution wherein D[3,2] is from about 5 to about 22.

[0048] It has been found that the present micronized com protein product is expected to be highly digestible, as shown by in vitro protein digestibility analysis in a 48 Hour Pepsin-Hydrochloric Acid Digestion Evaluation in accordance with ISO 6655. In this analysis, samples are digested with the pepsin-hydrochloric acid solution for 48 hours, the suspension is filtered and the nitrogen content is determined using the method described for the determination of soluble crude protein (ie. Digestible crude protein “CPdig”) in comparison to the total crude protein (soluble and insoluble crude protein - “CPtot”) in the sample. The percentage of soluble crude protein in comparison to the total crude protein is an indication of the digestibility of the protein product, and is reported as the 48 Hour Pepsin-Hydrochloric Acid Digestion Value using the units “% (CPdig / CPtot).”

[0049] In an aspect, the micronized corn protein product has a high content of soluble crude protein after 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 93% (CPdig / CPtot). In an aspect, the micronized corn protein product has a 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 95% (CPdig / CPtot).

[0050] In an aspect, the micronized com protein product has an oil binding capacity of from 1 to 1.3. For purposes of the present discussion, Oil Binding Capacity is defined as the amount of oil that is bound to the protein molecule, which is expressed in grams of oil held per gram of protein. The oil binding capacity of proteins is related to the protein’s surface hydrophobicity and its overall solubility. Oil binding capacity is generally measured by slowly adding oil to a set amount of protein and mixing until the protein is completely wetted. The mixture is centrifuged at a low speed and the oil that remains in the protein is weighed and calculated as the amount of oil that can be bound. The oil-binding capacity value as reported is an average of 2 measurements, and is expressed as g oil / g sample.

[0051] In an aspect, the micronized com protein product exhibits a pleasing mild yellow color. In an aspect, the micronized com protein product has an L*a*b* color measurement ofL* of from 70 to 85, a* of from -4 to 0, and b* of from 28 to 33.

[0052] The micronized corn protein product as described herein exhibits excellent dispersibility and stability characteristics as demonstrated in the Dispersibility (sedimentation) and Stability Evaluation discussion below. As can be seen in the data described therein, the micronized corn protein product is surprisingly dispersible and stable as compared to non-micronized corn protein and commercially available proteins used in milk replacer compositions. In particular, the micronized com protein product exhibits low sedimentation characteristics over time, facilitating mixing and feeding of animals without undue formation of sediment. Similarly, the micronized corn protein product exhibits low foaming characteristics, thereby providing a high ratio of available protein solution.

[0053] Alternative dispersibility and stability studies may be carried out using a Turbiscan™ Tower to characterize the nature and stability of micronized corn protein product in solutions. The Turbiscan™ Tower system advantageously provides accelerated testing to determine the sedimentation characteristics of the composition over the projected time of use.

[0054] The micronized corn protein product as described herein may be as a component in a milk replacer formulation, and particularly as a component in an animal milk replacer formulation.

[0055] The micronized corn protein product is incorporated in a dry milk replacer formulation in an amount suitable for providing the desired nutrition in a liquid milk replacer composition. For example, the micronized corn protein product may be present in a dry milk replacer formulation in an amount of from about 2% to about 5%, dry weight.

[0056] In an aspect, a dry milk replacer formulation may be prepared by mixing the micronized corn protein product as described herein with dry milk replacer ingredients comprising dairy proteins, carbohydrates, and fat.

[0057] In an aspect, a liquid milk replacer composition may be prepared by mixing the dry milk replacer formulation described herein with water in a quantity sufficient to provide a liquid milk replacer composition having a nutrition concentration level suitable for feeding an animal in need of such feeding.TEST METHODOLOGIESI. Particle Size Distribution

[0058] Particle size distribution is determined by laser diffraction techniques using the Mastersizer 3000 measurement instrument from Malvern Instruments Limited, as follows: Powder samples were dispersed in air in the AeroS module. Particles were defined in the software as non-spherical. Measurements were done in triplicate at a pressure of 2 bar while feeding witha feed rate of 45 %. The dispersant refractive index was set to 1, the particle refractive index toI.59 and the particle absorption index to 0.01. The hopper gap was set to 2.5 mm. Data were collected with obscuration level between 0.5 and 8%. The volumetric particle size distribution was calculated from the intensity profile of the scattered light with the Mie theory by use of the instrument’s software.II. Dispersibility (Sedimentation) and Stability Evaluation

[0059] Evaluation of the amount of Sedimentation of the protein additives is carried out using the following protocol:A, Sample preparation pH 4,5:

[0060] 100 g protein is mixed with 900 g of tap water at 45° in a 2000 ml beaker and stirred under 45 °C constant temperature for five minutes until all protein is dispersed.B, Sample preparation pH 6,2:

[0061] Standard milk replacer formulations comprise components such that the final liquid milk replacer composition is at a pH of about 6.2. Therefore, the solubility of the protein is evaluated at pH 6.2 to approximate conditions of use.

[0062] 100 g protein is mixed with 900 g of tap water (comprising sufficient sodium hydroxide to provide a solution having pH 6.2) at 45° in a 2000 ml beaker and stirred under 45 °C constant temperature for five minutes until all protein is dispersed.C, Stability Evaluation procedure

[0063] The resulting suspension is poured into the 1000 ml graduated cylinder for visual evaluation of foaming (visually apparent at top of cylinder) and sedimentation (visually apparent at bottom of cylinder). It is desirable to have a low amount of visually apparent sediment at the bottom of the cylinder. Likewise, is desirable to have a low amount of visually apparent foam at the top of the cylinder.

[0064] The volume of dispersed protein, which is the volume of liquid in the cylinder minus the volume of foam and the volume of sediment, is reported as a Stable Protein Solution Volume at identified times after mixing. Stability evaluations are carried out, for example, the time of mixing (TO) and 5, 15, and 30, and 60 minutes after mixing (T5, T15, T30 and T60). High Stable Protein Solution Volume values over time thus is an indication of the ability to deliver high amounts protein in the final milk replacer composition that will be consumed by the animal.

[0065] In an aspect, the Stable Protein Solution Volume at TO is greater than 800. In an aspect, the Stable Protein Solution Volume at TO is greater than 850. In an aspect, the Stable ProteinSolution Volume at TO is greater than 900. In an aspect, the Stable Protein Solution Volume at TO is greater than 950.

[0066] In an aspect, the Stable Protein Solution Volume at T5 is greater than 800. In an aspect, the Stable Protein Solution Volume at T5 is greater than 850. In an aspect, the Stable Protein Solution Volume at T5 is greater than 900. In an aspect, the Stable Protein Solution Volume at T5 is greater than 950.

[0067] In an aspect, the Stable Protein Solution Volume at T15 is greater than 800. In an aspect, the Stable Protein Solution Volume at T15 is greater than 850. In an aspect, the Stable Protein Solution Volume at T15 is greater than 900. In an aspect, the Stable Protein Solution Volume at T15 is greater than 950.

[0068] In an aspect, the Stable Protein Solution Volume at T30 is greater than 800. In an aspect, the Stable Protein Solution Volume at T30 is greater than 850. In an aspect, the Stable Protein Solution Volume at T30 is greater than 900. In an aspect, the Stable Protein Solution Volume at T30 is greater than 950.

[0069] In an aspect, the Stable Protein Solution Volume at T60 is greater than 800. In an aspect, the Stable Protein Solution Volume at T60 is greater than 850. In an aspect, the Stable Protein Solution Volume at T60 is greater than 900.EXAMPLESI. Preparation of materials for evaluationExample 1 Preparation of micronized CGM Sample A

[0070] A commercially available Corn Gluten Meal (corn gluten meal 13871 from Cargill) was micronized in a Hosokawa Milling machine to a particle size distribution as shown in Table 1. The particle size distribution was measured with laser diffraction using a Mastersizer 3000 from Malvern Instruments Limited.Table 1 - particle size distribution, micronized corn proteinExample 2 Preparation of micronized corn protein Sample B

[0071] Corn gluten meal 13871 was micronized in a ZPS impact mill with integrated ALPINE Turboplex Ultrafine Classifier ATP by Hosokawa Alpine to a particle size distribution as shown in Table 2. The particle size distribution was measured with laser diffraction using a Mastersizer 3000 from Malvern Instruments Limited.Table 2 - particle size distribution, micronized corn proteinExample 3 Preparation of Comparative Corn Gluten Meal (“CGM”)

[0072] A commercially available Corn Gluten Meal (corn gluten meal 13871 from Cargill) was obtained for evaluation, but not micronized. The corn gluten meal had a particle distribution as shown in Table 3. The particle size distribution was measured with laser diffraction using a Mastersizer 3000 from Malvern Instruments Limited.Table 3 - particle size distribution, Corn Gluten MealExample 4 Preparation of Comparative Soy Bean Protein (“SBP”) Sample

[0073] A commercially available soy bean meal that is a protein concentrate product used as a component in Calf Milk Replacers was obtained for comparison purposes.Example 5 Preparation of Comparative Hydrolyzed Wheat Protein (“HWP”) Sample

[0074] A commercially available hydrolyzed wheat protein product that is used as a component in Calf Milk Replacers, C*HyProw® hydrolyzed wheat protein from Cargill, was obtained for comparison purposes.II. Material EvaluationA. Dispersibility and Stability

[0075] Dispersibility (Sedimentation) and Stability of the above samples of Examples 1-5 were evaluated using the methodology described above, wherein the results are reported as Stable Protein Solution Volume.Table 4 - Stable Protein Solution Volume at pH 4.5Table 5 - Stable Protein Solution Volume at pH 6.2Table 6 - Stable Protein Solution Volume at pH 4.5Table 7 - Stable Protein Solution Volume at pH 6.2Table 8 - Stable Protein Solution Volume at pH 4.5Table 9 - Stable Protein Solution Volume at pH 6.2

[0076] The Stable Protein Solution Volume for this material was evaluated as described above with the following result:Table 10 - Stable Protein Solution Volume at pH 4.5Table 11 - Stable Protein Solution Volume at pH 6.2Table 12 - Stable Protein Solution Volume at pH 4.5Table 13 - Stable Protein Solution Volume at pH 6.2B. Digestibility

[0077] Digestibility of the above samples of Examples 1-5 were evaluated using the methodology of the 48 Hour Pepsin-Hydrochloric Acid Digestion Evaluation in accordance with ISO 6655 described above, reported in Table 14:Table 14, digestibilityDISCUSSION OF EXAMPLES 1-5

[0078] It has been found that corn gluten meal that has been micronized as described herein surprisingly exhibits excellent stability in solution as compared to corn gluten meal that has not been micronized. Moreover, the stability of the protein solution as evaluated and reported as Stable Protein Solution Volume surprisingly meets or exceeds the performance of commercially available protein products that are currently used in Calf Milk Replacer formulations. The data presented in Tables 3-12 is graphically represented in FIG. 1, which shows the Stable Protein Solution Volume at pH 4.5 (typically the pH of preparation and storage of the protein compositions) and at pH 6.2 (typically the pH of the ultimate milk replacer composition).

[0079] It additionally was found that corn gluten meal that has been micronized as described herein surprisingly exhibits excellent digestibility as predicted by the 48 Hour Pepsin- Hydrochloric Acid Digestion Evaluation. It is noted that the test protocol set forth in ISO 6655 required 48 hours of incubation in the Pepsin-Hydrochloric Acid. Since protein digestion in calves is ordinarily completed in only 24 hours, the relative superiority of digestibility of the micronized corn gluten meal as compared to other tested protein sources is expected to be even greater in vivo.

[0080] The stability of the micronized com gluten meal as compared to conventional corn gluten meal, in combination with the superior digestibility of the micronized corn gluten meal as compared to conventional com gluten meal provides unique and efficient addition of a naturally sourced corn protein product in a final milk replacer formulation.

[0081] The presently described micronized corn protein product advantageously permits use of a new category of protein source for use in milk replacer formulations, with performance that meets or exceeds the performance of commercially available protein products currently being used.EXAMPLE 6: CALF TRIAL

[0082] This trial is designed to compare four different protein sources in milk replacers for calves. Soy protein (Soycomil R), Hydrolyzed wheat protein, and two different micronized corn protein products having different particle size distributions. Corn protein 2 and Corn protein 3 are micronized corn protein products according to the invention described herein (having a particle size distribution wherein dlO is from about 3 to about 9 microns, d50 is from about 8 to about 35 microns, d90 is from about 15 to about 70 microns, and d99 is from about 80 to about 95 microns;a protein content of at least about 50% dry weight; and a moisture content of less than about 14% or having a particle size distribution wherein dlO is from about 3 to about 10 microns, d50 is from about 8 to about 45 microns, and d90 is from about 15 to about 99 microns; a protein content of at least about 50% dry weight; and a moisture content of less than about 14%).Materials and Methods

[0083] A total of ~80 dairy beef male / female from calves 7 to 14 days of age (Angus x Holstein; Holstein) are used in the trial. Calves arrive from dairy farms in batches of approximately 10 to 15 animals.

[0084] Calves are allocated in a partially opened barn with 8 pens (10 animals / pen) bedded with straw or sawdust. Each pen is equipped with an automatic milk feeder and automatic concentrate feeder.

[0085] At arrival calves are weighed (BW), and a thoracic ultrasonography is performed to all calves. Lung lesions observed with the ultrasound is scored on a scale of 1 to 4 based on findings within the entire lung field (Ollivett et al., 2015). Briefly, a score of 1 is attributed to calves with no abnormalities, meaning only a healthy pleural surface or isolated comet tail within an image field. A score of 2 is given if comet tails on the pleural surface were multiple and B-lines (coalescence of multiple comet tails) without significant lung consolidation are observed. A score of 3 is assigned to calves with one or more locations of lung consolidation > 1 cm. A score of 4 is assigned to calves with extensive consolidation (> 6 cm in one or more locations), abscess within the lung parenchyma seen as an encapsulated fluid filled space, or significant pleural effusion. The ultrasound score is used together with the BW to randomize calves among treatments.

[0086] The feeding program is provided in Table 15 and the Milk Replacer Formulations are provided in Table 16. Particle size data for Corn protein 2 and Corn protein is in Table 17.Table 15: Calf Trial Feeding ProgramTable 16: Milk Replacer Formulations for Calf TrialTable 17: Particle Size DistributionDigestibility

[0087] A subset of 40 calves (10 calves / treatment) is used to evaluate apparent total tract digestibility. Calves are fed chromic oxide at a rate of Ig / Kg of DM (1.5 g / kg of FM). Digestibility test is performed in two different periods at the end of week 3 and of week 8. At week 8 chromic oxide is added to the concentrate feed too at the same rate.

[0088] Calves are fed Cr2O3 for 7 days and the last 3 days fecal samples are collected 5 times a day by rectal estimulation. Samples are kept in a fridge until the end of the day so that all pulls are frozen together each day.

[0089] Before sending the fecal samples to analyze, samples are thawed and create a unique sample from the 3 collection days.Results

[0090] Calves entered into the study in 6 different batches (weeks), 14 days of data from all calves have been included in the analysis, except the dead ones that have been removed from the analysis. No differences have been observed among treatment (P = 0.96) nor treatment by time interaction (P = 0.94; Figure 3) on body weight during the first 14 days of study.

[0091] Results showed a treatment by time interaction on calf milk replacer intake for the first 14 days of the study (P < 0.01; Figure 4). During the first 3 days of the study calves fed milk replacer with Corn protein 2 and Corn protein 3 had lower intake of milk replacer than calves fed milkreplacer with Soycomil or Hydrolysed Wheat Protein. After the first 3 days all calves had similar intake among treatments.

[0092] Drinking speed was also affected by treatment (P = 0.04, Figure 5) in which calves fed CMR (Calf Milk Replacer) with Soycomil had faster drinking speeds than calves fed Com Protein 3, while calves fed CMR with Hydrolysed wheat protein and Corn Protein 2 where intermediate. Although all calves are fed the same concentrate feed, a treatment effect (P < 0.01; Figure 6) was observed for it. Calves fed Corn Protein 3 are eating more concentrate feed than the rest of the treatments, followed by calves fed Soycomil.ADDITIONAL EXAMPLES

[0093] The following examples are non-limiting examples of the invention described herein.

[0094] Example 1. A micronized corn protein product having a particle size distribution wherein dlO is from about 3 to about 9 microns, d50 is from about 8 to about 35 microns, d90 is from about 15 to about 70 microns, and d99 is from about 80 to about 95 microns; a protein content of at least about 50% dry weight; and a moisture content of less than about 14%.

[0095] Example 2. The micronized com protein product of example 1, wherein the micronized corn protein product has a particle size distribution wherein dlO is from about 4 to about 8 microns, d50 is from about 9 to about 30 microns, d90 is from about 17 to about 65 microns, and d99 is from about 80 to about 95 microns.

[0096] Example 3. The micronized com protein product of example 1, wherein the micronized corn protein product has a particle size distribution wherein D[3,2] is from about 5 to about 20.

[0097] Example 4. The micronized com protein product of example 1, wherein the micronized corn protein product has a particle size distribution wherein D[4,3] is from about 8 to about 40.

[0098] Example 5. The micronized corn protein product of any one of the preceding examples, wherein the micronized corn protein product has a protein content of from about 50% to about 98% dry weight; or wherein the micronized com protein product has a protein content of from about 50% to about 65% dry weight; or wherein the micronized corn protein product has a protein content of from about 65% to about 85 dry weight; or wherein the micronized corn protein product has a protein content of from about 85% to about 98 dry weight.

[0099] Example 6. The micronized corn protein product of any one of the preceding examples, wherein the micronized com protein product has a moisture content of less than about 12%; or wherein the micronized com protein product has a moisture content of less than about 10%; or wherein the micronized com protein product has a moisture content of less than about 8%;orwherein the micronized corn protein product has a moisture content of less than about 6%; or wherein the micronized corn protein product has a moisture content of from about 3.5% to about 8%.

[0100] Example 7. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at TO is greater than 800; or wherein the Stable Protein Solution Volume at TO is greater than 850; or wherein the Stable Protein Solution Volume at TO is greater than 900; or wherein the Stable Protein Solution Volume at TO is greater than 950.

[0101] Example 8. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at Volume at T5 is greater than 800. In an aspect, the Stable Protein Solution Volume at T5 is greater than 850. In an aspect, the Stable Protein Solution Volume at T5 is greater than 900. In an aspect, the Stable Protein Solution Volume at T5 is greater than 950.

[0102] Example 9. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at T15 is greater than 800; or wherein the Stable Protein Solution Volume at T15 is greater than 850; or wherein the Stable Protein Solution Volume at T 15 is greater than 900; or wherein the Stable Protein Solution Volume at T15 is greater than 950.

[0103] Example 10. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at T30 is greater than 800; or wherein the Stable Protein Solution Volume at T30 is greater than 850; or wherein the Stable Protein Solution Volume at T30 is greater than 900; or wherein the Stable Protein Solution Volume at T30 is greater than 950.

[0104] Example 11. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at T60 is greater than 800; or wherein the Stable Protein Solution Volume at T60 is greater than 850; or wherein the Stable Protein Solution Volume at T60 is greater than 900.

[0105] Example 12. The micronized corn protein product of any one of the preceding examples, wherein the micronized corn protein product has a 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 93% (CPdig / CPtot); or wherein the micronized corn protein product has a 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 95% (CPdig / CPtot).

[0106] Example 13. The micronized corn protein product of any one of the preceding examples, wherein the micronized com protein product has an oil binding capacity of from 1 to 1.3.

[0107] Example 14. The micronized corn protein product of any one of the preceding examples, wherein the micronized corn protein product has an L*a*b* color measurement of L* of from 70 to 85, a* of from -4 to 0, and b* of from 28 to 33.

[0108] Example 15. The micronized corn protein product of any one of examples 1-14 for use as a component in a dry milk replacer formulation.

[0109] Example 16. The micronized corn protein product of any one of examples 1-14 for use as a component in a liquid milk replacer composition.

[0110] Example 17. A dry milk replacer formulation comprising the micronized corn protein product of any one of examples 1-14.

[0111] Example 18. The dry milk replacer formulation of example 17, wherein the micronized corn protein product is present in a dry milk replacer formulation in an amount of from about 2% to about 5%, dry weight.

[0112] Example 19. A method of making a dry milk replacer formulation comprising mixing the micronized corn protein product of any one of examples 1-14 with dry milk replacer ingredients comprising dairy proteins, carbohydrates, and fat.

[0113] Example 20. A method of feeding an animal, comprising feeding the animal a milk replacer comprising the micronized corn protein product of any one of examples 1-14.

[0114] Example 21. A method of feeding an animal, comprising feeding the animal a milk replacer formulation according to any one of examples 17-18.

[0115] Example 22. The method of any one of examples 20 or 21, wherein the milk replacer or milk replacer formulation is fed to an animal starting at 7 to 14 days of age.

[0116] Example 23. The method of any one of examples 20-22, wherein the milk replacer or milk replacer formulation is fed to the animal for 1 to 30 days; for 1 to 65 days; for 1 to 75 days; for 1 to 90 days; for 65 to 75 days; or for 30 to 90 days post-birth.

[0117] Example 24. The method or use of any of the preceding claims, wherein the animal is a calf.

[0118] Example 25. A micronized corn protein product having a particle size distribution wherein dlO is from about 3 to about 10 microns, d50 is from about 8 to about 45 microns, and d90 is from about 15 to about 99 microns; a protein content of at least about 50% dry weight; and a moisture content of less than about 14%.

[0119] Example 26. The micronized corn protein product of example 25, wherein the micronized corn protein product has a particle size distribution wherein dlO is from about 4 to about 9 microns, d50 is from about 9 to about 44 microns, and d90 is from about 20 to about 98 microns.

[0120] Example 27. The micronized corn protein product of example 25, wherein the micronized corn protein product has a particle size distribution wherein D[3,2] is from about 5 to about 22.

[0121] Example 28. The micronized corn protein product of example 25, wherein the micronized corn protein product has a particle size distribution wherein D[4,3] is from about 8 to about 50.

[0122] Example 29. The micronized corn protein product of any one of the preceding examples, wherein the micronized corn protein product has a protein content of from about 50% to about 98% dry weight; or wherein the micronized com protein product has a protein content of from about 50% to about 65% dry weight; or wherein the micronized corn protein product has a protein content of from about 65% to about 85 dry weight; or wherein the micronized corn protein product has a protein content of from about 85% to about 98 dry weight.

[0123] Example 30. The micronized corn protein product of any one of the preceding examples, wherein the micronized com protein product has a moisture content of less than about 12%; or wherein the micronized com protein product has a moisture content of less than about 10%; or wherein the micronized com protein product has a moisture content of less than about 8%;or wherein the micronized corn protein product has a moisture content of less than about 6%; or wherein the micronized corn protein product has a moisture content of from about 3.5% to about 8%.

[0124] Example 31. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at TO is greater than 800; or wherein the Stable Protein Solution Volume at TO is greater than 850; or wherein the Stable Protein Solution Volume at TO is greater than 900; or wherein the Stable Protein Solution Volume at TO is greater than 950.

[0125] Example 32. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at Volume at T5 is greater than 800. In an aspect, the Stable Protein Solution Volume at T5 is greater than 850. In an aspect, the Stable Protein Solution Volume at T5 is greater than 900. In an aspect, the Stable Protein Solution Volume at T5 is greater than 950.

[0126] Example 33. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at T15 is greater than 800; or wherein the Stable Protein Solution Volume at T15 is greater than 850; or wherein the Stable Protein Solution Volume at T 15 is greater than 900; or wherein the Stable Protein Solution Volume at T15 is greater than 950.

[0127] Example 34. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at T30 is greater than 800; or wherein the StableProtein Solution Volume at T30 is greater than 850; or wherein the Stable Protein Solution Volume at T30 is greater than 900; or wherein the Stable Protein Solution Volume at T30 is greater than 950.

[0128] Example 35. The micronized corn protein product of any one of the preceding examples, wherein the Stable Protein Solution Volume at T60 is greater than 800; or wherein the Stable Protein Solution Volume at T60 is greater than 850; or wherein the Stable Protein Solution Volume at T60 is greater than 900.

[0129] Example 36. The micronized corn protein product of any one of the preceding examples, wherein the micronized corn protein product has a 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 93% (CPdig / CPtot); or wherein the micronized corn protein product has a 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 95% (CPdig / CPtot).

[0130] Example 37. The micronized corn protein product of any one of the preceding examples, wherein the micronized com protein product has an oil binding capacity of from 1 to 1.3.

[0131] Example 38. The micronized corn protein product of any one of the preceding examples, wherein the micronized corn protein product has an L*a*b* color measurement of L* of from 70 to 85, a* of from -4 to 0, and b* of from 28 to 33.

[0132] Example 39. The micronized corn protein product of any one of examples 1-14 for use as a component in a dry milk replacer formulation.

[0133] Example 40. The micronized corn protein product of any one of examples 1-14 for use as a component in a liquid milk replacer composition.

[0134] Example 41. A dry milk replacer formulation comprising the micronized corn protein product of any one of examples 25-38.

[0135] Example 42. The dry milk replacer formulation of example 17, wherein the micronized corn protein product is present in a dry milk replacer formulation in an amount of from about 2% to about 5%, dry weight.

[0136] Example 43. A method of making a dry milk replacer formulation comprising mixing the micronized corn protein product of any one of examples 25-38 with dry milk replacer ingredients comprising dairy proteins, carbohydrates, and fat.

[0137] Example 44. A method of feeding an animal, comprising feeding the animal a milk replacer comprising the micronized corn protein product of any one of examples 25-38.

[0138] Example 45. A method of feeding an animal, comprising feeding the animal a milk replacer formulation according to any one of examples 41-42.

[0139] Example 46. The method of any one of examples 44 or 45, wherein the milk replacer or milk replacer formulation is fed to an animal starting at 7 to 14 days of age.

[0140] Example 47. The method of any one of examples 44 to 46, wherein the milk replacer or milk replacer formulation is fed to the animal for 1 to 30 days; for 1 to 65 days; for 1 to 75 days; for 1 to 90 days; for 65 to 75 days; or for 30 to 90 days post-birth.

[0141] Example 48. The method or use of any of the preceding claims, wherein the animal is a calf.

[0142] As used herein, the terms "about" or "approximately" mean within an acceptable range for the particular parameter specified as determined by one of ordinary skill in the art, which will depend in part on how the value is measured or determined, e.g., the limitations of the sample preparation and measurement system. Examples of such limitations include preparing the sample in a wet versus a dry environment, different instruments, variations in sample height, and differing requirements in signal -to-noise ratios.

[0143] All patents, patent applications (including provisional applications), and publications cited herein are incorporated by reference as if individually incorporated for all purposes. Unless otherwise indicated, all parts and percentages are by weight and all molecular weights are weight average molecular weights. The foregoing detailed description has been given for clarity of understanding only. No unnecessary limitations are to be understood therefrom. The invention is not limited to the exact details shown and described, for variations obvious to one skilled in the art will be included within the invention defined by the claims.

Claims

WHAT IS CLAIMED IS:

1. A micronized corn protein product having a particle size distribution wherein dlO is from about 3 to about 9 microns, d50 is from about 8 to about 35 microns, d90 is from about 15 to about 70 microns, and d99 is from about 80 to about 95 microns; a protein content of at least about 50% dry weight; and a moisture content of less than about 14%.

2. The micronized com protein product of claim 1, wherein the micronized com protein product has a particle size distribution wherein dlO is from about 4 to about 8microns, d50 is from about 9 to about 30 microns, d90 is from about 17 to about 65 microns, and d99 is from about 80 to about 95 microns.

3. The micronized com protein product of claim 1, wherein the micronized com protein product has a particle size distribution wherein D[3,2] is from about 5 to about 20.

4. The micronized com protein product of claim 1, wherein the micronized com protein product has a particle size distribution wherein D[4,3] is from about 8 to about 40.

5. The micronized corn protein product of any one of the preceding claims, wherein the micronized com protein product has a protein content of from about 50% to about 98% dry weight; or wherein the micronized corn protein product has a protein content of from about 50% to about 65% dry weight; or wherein the micronized com protein product has a protein content of from about 65% to about 85 dry weight; or wherein the micronized corn protein product has a protein content of from about 85% to about 98 dry weight.

6. The micronized corn protein product of any one of the preceding claims, wherein the Stable Protein Solution Volume at TO is greater than 800; or wherein the Stable Protein SolutionVolume at TO is greater than 850; or wherein the Stable Protein Solution Volume at TO is greater than 900; or wherein the Stable Protein Solution Volume at TO is greater than 950.

7. The micronized corn protein product of any one of the preceding claims, wherein the Stable Protein Solution Volume at Volume at T5 is greater than 800. In an aspect, the Stable Protein Solution Volume at T5 is greater than 850. In an aspect, the Stable Protein Solution Volume at T5 is greater than 900. In an aspect, the Stable Protein Solution Volume at T5 is greater than 950.

8. The micronized corn protein product of any one of the preceding claims, wherein the Stable Protein Solution Volume at T15 is greater than 800; or wherein the Stable Protein Solution Volume at T15 is greater than 850; or wherein the Stable Protein Solution Volume at T15 is greater than 900; or wherein the Stable Protein Solution Volume at T15 is greater than 950.

9. The micronized com protein product of any one of the preceding claims, wherein the Stable Protein Solution Volume at T30 is greater than 800; or wherein the Stable Protein Solution Volume at T30 is greater than 850; or wherein the Stable Protein Solution Volume at T30 is greater than 900; or wherein the Stable Protein Solution Volume at T30 is greater than 950.

10. The micronized corn protein product of any one of the preceding claims, wherein the Stable Protein Solution Volume at T60 is greater than 800; or wherein the Stable Protein Solution Volume at T60 is greater than 850; or wherein the Stable Protein Solution Volume at T60 is greater than 900.

11. The micronized com protein product of any one of the preceding claims, wherein the micronized com protein product has a 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 93% (CPdig / CPtot); or wherein the micronized com protein product has a 48 Hour Pepsin-Hydrochloric Acid Digestion of at least 95% (CPdig / CPtot).

12. The micronized corn protein product of any one of the preceding claims, wherein the micronized com protein product has an oil binding capacity of from 1 to 1.3.

13. The micronized corn protein product of any one of claims 1-12 for use as a component in a dry milk replacer formulation or a liquid milk replacer composition.

14. A dry milk replacer formulation comprising the micronized corn protein product of any one of claims 1-12.

15. The dry milk replacer formulation of claim 14, wherein the micronized com protein product is present in a dry milk replacer formulation in an amount of from about 2% to about 5%, dry weight.

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