AU2024324023B2

AU2024324023B2 - Dairy product and process

Info

Publication number: AU2024324023B2
Application number: AU2024324023A
Authority: AU
Inventors: Piratheepan Mahendran
Original assignee: Fonterra Cooperative Group Ltd
Current assignee: Fonterra Cooperative Group Ltd
Priority date: 2023-08-14
Filing date: 2024-08-14
Publication date: 2025-10-16
Anticipated expiration: 2044-08-14
Also published as: WO2025037250A1; AU2024324023A1; TW202510744A

Abstract

The present invention relates to frozen milk concentrates, and methods for producing such frozen milk concentrates.

Description

WO 2025/037250 A1 Published: with with international international search search report report (Art. (Art. 21(3)) 21(3))

- before the expiration of the time limit for amending the

- claims and to be republished in the event of receipt of amendments (Rule 48.2(h))

DAIRY PRODUCT AND PROCESS FIELD OF THE INVENTION

[001] The present invention relates to frozen milk concentrates, and methods of producing frozen milk concentrates. 2024324023

[002] The frozen milk concentrates described herein have high total solids and/or total protein content. The frozen milk concentrates described herein may be thawed, diluted and any aggregates readily broken down by standard processing to form liquid milk products having one or more of the following properties: an acceptable flavour profile, low sedimentation, small particle size, a stable milk colloidal system and no undesirable aggregation, gelling and/or grittiness. Favourably, the frozen milk concentrates described herein may retain one or more of these properties following storage at -18 °C or less for prolonged periods up to 24 months. Furthermore, the process described herein may be more energy efficient than existing processes.

BACKGROUND TO THE INVENTION

[003] In various locations worldwide the demand for products made from fresh milk outstrips the local fresh milk supply. While reconstituted milk powder can be used, consumers do not always accept the powder flavour notes of such products. Frozen milk concentrates provide an alternative with a fresh milk flavour, but the current offerings are expensive to produce due to the concentration and freezing technologies employed.

[004] There is an ongoing need for frozen concentrated milk products with high protein and/or total solids content that are produced by efficient, scalable methods.

[005] It is an object of the present invention to go some way to meeting this need; and/or to at least provide the public with a useful choice.

[006] Other objects of the invention may become apparent from the following description which is given by way of example only.

[007] Any discussion of documents, acts, materials, devices, articles, or the like which has been included in the present specification is solely for the purpose of providing a context for the present invention. It is not to be taken as an admission that any or all of these matters form part of the prior art base or were common general knowledge in the field relevant to the present invention as it existed before the priority date.

SUMMARY OF THE INVENTION

[007a] In a first aspect the invention provides a frozen milk concentrate comprising from about 14% to about 35% by weight total protein and at least about 20% by weight total milk solids, wherein the total protein comprises β-lactoglobulin of which less than about 40% by weight is denatured, and wherein from about 45 to about 90% of total 2024324023

milk solids-not-fat in the frozen milk concentrate is protein.

[007b] In a second aspect the invention provides a frozen milk concentrate comprising at least about 51% by weight total milk solids and at least about 12% by weight total protein, wherein total protein in the frozen milk concentrate comprises β-lactoglobulin of which less than about 40% by weight is denatured.

[007c] In a third aspect the invention provides a process for preparing a frozen milk concentrate, the process comprising

a) heating liquid milk to a temperature of from about 30°C to about 100°C for less than about 60 seconds to provide a heated milk composition,

b) providing an evaporation system that comprises a falling film evaporator and optionally a thin film evaporator,

c) removing moisture from the heated milk composition through evaporative processing using the evaporation system to produce a concentrated milk comprising at least about 51% total milk solids and at least about 12% by weight total protein,

d) cooling the concentrated milk under shear to a temperature of less than 10°C to provide a cooled milk concentrate, and

e) freezing the cooled milk concentrate to a temperature of less than about - 10°C, preferably less than about -18°C, to provide a frozen milk concentrate;

wherein the evaporation system is operated at a temperature of from about 40°C to about 70°C.

[007d] In a fourth aspect the invention provides a process for preparing a frozen milk concentrate, the process comprising

a) providing a milk protein concentrate (MPC) comprising at least about 15% by weight total solids and at least about 12% by weight total protein, 2024324023

b) heating the MPC to a temperature of from about 30°C to about 100°C for less than about 60 seconds to provide a heated MPC,

c) providing an evaporation system that comprises a falling film evaporator and optionally a thin film evaporator,

d) removing moisture from the heated MPC through evaporative processing using the evaporation system to produce a concentrated milk comprising at least about 14% by weight total protein and at least about 20% by weight total solids,

e) cooling the concentrated milk under shear to a temperature of less than 10°C to provide a cooled milk concentrate, and

f) freezing the cooled milk concentrate to a temperature of less than about - 10°C, preferably less than about -18°C, to provide a frozen milk concentrate;

wherein the evaporation system is operated at a temperature of from about 40°C to about 70°C; and optionally with a shear rate of at least about 10 s-1.

[007e] In a fifth aspect the invention provides a frozen milk concentrate obtained by the process of the third or fourth aspects.

[007f] Certain statements that appear below are broader than what appears in the statements of the invention above. These statements are provided in the interests of providing the reader with a better understanding of the invention and its practice. The reader is directed to the accompanying claim set which defines the scope of the invention.

[008] In one aspect, the present invention provides a frozen milk concentrate comprising from about 14% to about 35% by weight total protein and at least about 20%

by weight total milk solids, wherein the total protein comprises β-lactoglobulin of which less than about 40% by weight is denatured.

[009] In one aspect, the invention provides a frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein total protein in the frozen milk concentrate comprises β-lactoglobulin of which less than about 40% by weight is denatured. 2024324023

[0010] In one aspect, the present invention provides a frozen milk concentrate comprising from about 14% to about 35% by weight total protein and at least about 20% by weight total milk solids, wherein the total protein comprises denaturable whey protein of which less than about 40% by weight is denatured.

[0011] In one aspect, the invention provides a frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein total protein in the frozen milk concentrate comprises denaturable whey protein of which less than about 40% by weight is denatured.

[0012] In one aspect, the present invention provides a frozen milk concentrate comprising from about 14% to about 35% by weight total protein and at least about 20% by weight total milk solids, wherein the total protein comprises lactoferrin of which less than about 95% by weight is denatured; or wherein the frozen milk concentrate comprises at least about 0.1 mg native (undenatured) lactoferrin per gram of total protein.

[0013] In one aspect, the invention provides a frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein total protein in the frozen milk concentrate comprises lactoferrin of which less than about 95% by weight is denatured; or wherein the frozen milk concentrate comprises at least about 0.1 mg native (undenatured) lactoferrin per gram of total protein.

[0014] In one aspect, the invention provides a process for preparing a frozen milk concentrate, the process comprising

i) heating liquid milk to a temperature of from about 30°C to about 100°C for less than about 240 seconds to provide a heated milk composition,

ii) providing an evaporation system that comprises a falling film evaporator and optionally a thin film evaporator,

iii) removing moisture from the heated milk composition through evaporative processing using the evaporation system to produce a concentrated milk comprising at least about 51% total milk solids,

iv) cooling the concentrated milk under shear to a temperature of less than 10°C to provide a cooled milk concentrate, and 2024324023

v) freezing the cooled milk concentrate to a temperature of less than about - 10°C, preferably less than about -18°C, to provide a frozen milk concentrate;

[0015] In one aspect, the invention provides a process for preparing a frozen milk concentrate, the process comprising

i) providing a milk protein concentrate (MPC) comprising at least about 15% by weight total solids and at least about 12% by weight total protein,

ii) heating the MPC to a temperature of from about 30°C to about 100°C for less than about 60 seconds to provide a heated MPC,

iii) providing an evaporation system that comprises a falling film evaporator and/or a thin film evaporator,

iv) removing moisture from the heated MPC through evaporative processing using the evaporation system to produce a concentrated milk comprising at least about 14% by weight total protein and at least about 20% by weight total solids,

v) cooling the concentrated milk under shear to a temperature of less than 10°C to provide a cooled milk concentrate, and

vi) freezing the cooled milk concentrate to a temperature of less than about - 10°C, preferably less than about -18°C, to provide a frozen milk concentrate;

[0016] In one aspect, the invention provides a frozen milk concentrate obtained by the process of the invention.

[0017] In one aspect, the invention provides a frozen milk concentrate obtainable by the process of the invention.

[0018] The following embodiments and preferences may relate alone or in any 2024324023

combination of any two or more to any of the above aspects.

[0019] In various embodiments, the frozen milk concentrate comprises at least about 12% by weight total protein.

[0020] In various embodiments, the frozen milk concentrate may comprise β- lactoglobulin of which less than about 40%, 39%, 38%, 37%, 36%, 35%, 34%, 33%, 32%, 31%, 30%, 28%, 26%, 25%, 24%, 23%, 22%, 21%, 20%, 19%, 18%, 17%, 16%, 15%, 12%, 10% by weight is denatured, and various ranges may be selected from between any two of these values, for example from about 0.1% to about 40%, or about 1% to about 40%, or about 2% to about 40%, or about 5% to about 40%, or about 8% to about 40%, or about 10% to about 40%, from about 0.1% to about 38%, or about 1% to about 38%, or about 2% to about 38%, or about 5% to about 38%, or about 8% to about 38%, or about 10% to about 38%, from about 0.1% to about 36%, or about 1% to about 36%, or about 2% to about 36%, or about 5% to about 36%, or about 8% to about 36%, or about 10% to about 36%, or about 12% to about 36%, or about 15% to about 36%, from about 0.1% to about 35%, or about 1% to about 35%, or about 2% to about 35%, or about 5% to about 35%, or about 8% to about 35%, or about 10% to about 35%, or about 12% to about 35%, or about 15% to about 35%, from about 0.1% to about 32%, or about 1% to about 32%, or about 2% to about 32%, or about 5% to about 32%, or about 8% to about 32%, or about 10% to about 32%, or about 12% to about 32%, or about 15% to about 32%, from about 0.1% to about 30%, or about 1% to about 30%, or about 2% to about 30%, or about 5% to about 30%, or about 8% to about 30%, or about 10% to about 30%, or about 12% to about 30%, or about 15% to about 30%, or about 0.1% to about 28%, or about 1% to about 28%, or about 2% to about 28%, or about 5% to about 28%, or about 8% to about 28%, or about 10% to about 28%, or about 12% to about 28%, or about 15% to about 28%, about 0.1% to about 25%, or about 1% to about 25%, or about 2% to about 25%, or about 5% to about 25%, or about 8% to about 25%, or about 10% to about 25%, or about 12% to about 25%, or about 15% to about 25%, about 0.1% to about 20%, or about 1% to about 20%, or about 2% to about 20%, or about 5% to about 20%, or about 8% to

about 20%, or about 10% to about 20%, or about 12% to about 20%, or about 15% to about 20% by weight is denatured.

[0021] In various embodiments the frozen milk concentrate may comprise at least about 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5 or 12 mg of native (undenatured) β-lactoglobulin per 100 g of total protein, and various ranges may be selected from between any two of these values, for example, from about 5 to about 12, 2024324023

about 5 to about 11, about 5 to about 10, about 5.5 to about 12, about 5.5 to about 11, about 5.5 to about 10, about 6 to about 12, about 6 to about 11, or about 6 to about 10 mg of native (undenatured) β-lactoglobulin per 100 g of total protein.

[0022] In various embodiments, the frozen milk concentrate may comprise denaturable whey protein of which less than about 40%, 39%, 38%, 37%, 36%, 35%, 34%, 33%, 32%, 31%, 30%, 28%, 26%, 25%, 24%, 23%, 22%, 21%, 20%, 19%, 18%, 17%, 16%, 15%, 12%, 10% by weight is denatured, and various ranges may be selected from between any two of these values, for example from about 0.1% to about 40%, or about 1% to about 40%, or about 2% to about 40%, or about 5% to about 40%, or about 8% to about 40%, or about 10% to about 40%, from about 0.1% to about 38%, or about 1% to about 38%, or about 2% to about 38%, or about 5% to about 38%, or about 8% to about 38%, or about 10% to about 38%, from about 0.1% to about 36%, or about 1% to about 36%, or about 2% to about 36%, or about 5% to about 36%, or about 8% to about 36%, or about 10% to about 36%, or about 12% to about 36%, or about 15% to about 36%, from about 0.1% to about 35%, or about 1% to about 35%, or about 2% to about 35%, or about 5% to about 35%, or about 8% to about 35%, or about 10% to about 35%, or about 12% to about 35%, or about 15% to about 35%, from about 0.1% to about 32%, or about 1% to about 32%, or about 2% to about 32%, or about 5% to about 32%, or about 8% to about 32%, or about 10% to about 32%, or about 12% to about 32%, or about 15% to about 32%, from about 0.1% to about 30%, or about 1% to about 30%, or about 2% to about 30%, or about 5% to about 30%, or about 8% to about 30%, or about 10% to about 30%, or about 12% to about 30%, or about 15% to about 30%, or about 0.1% to about 28%, or about 1% to about 28%, or about 2% to about 28%, or about 5% to about 28%, or about 8% to about 28%, or about 10% to about 28%, or about 12% to about 28%, or about 15% to about 28%, about 0.1% to about 25%, or about 1% to about 25%, or about 2% to about 25%, or about 5% to about 25%, or about 8% to about 25%, or about 10% to about 25%, or about 12% to about 25%, or about 15% to about 25%, about 0.1% to about 20%, or about 1% to about 20%, or about 2% to about 20%, or about 5% to about

20%, or about 8% to about 20%, or about 10% to about 20%, or about 12% to about 20%, or about 15% to about 20% by weight is denatured.

[0023] In various embodiments, the frozen milk concentrate may comprise lactoferrin, of which less than about 95% by weight is denatured, for example less than about 95%, 90%, 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%, 45%, 40%, 35%, 30%, 25%, 20%, 15%, 10%, or less than about 5% by weight is denatured, and various 2024324023

ranges may be selected from between any two of these values, for example from about 1% to about 95%, or about 2% to about 95%, or about 5% to about 95%, or about 10% to about 95%, or about 20% to about 95%, or about 30% to about 95%, or about 40% to about 95%, or about 50% to about 95%, or about 60% to about 95%, or about 70% to about 95%, or about 80% to about 95%, or from about 1% to about 90%, or about 2% to about 90%, or about 5% to about 90%, or about 10% to about 90%, or about 20% to about 90%, or about 30% to about 90%, or about 40% to about 90%, or about 50% to about 90%, or about 60% to about 90%, or about 70% to about 90%, or about 80% to about 90%, or from about 1% to about 80%, or about 2% to about 80%, or about 5% to about 80%, or about 10% to about 80%, or about 20% to about 80%, or about 30% to about 80%, or about 40% to about 80%, or about 50% to about 80%, or about 60% to about 80%, or about 70% to about 80%, from about 1% to about 70%, or about 2% to about 70%, or about 5% to about 70%, or about 10% to about 70%, or about 20% to about 70%, or about 30% to about 70%, or about 40% to about 70%, or about 50% to about 70%, or about 60% to about 70%, from about 1% to about 60%, or about 2% to about 60%, or about 5% to about 60%, or about 10% to about 60%, or about 20% to about 60%, or about 30% to about 60%, or about 40% to about 60%, or about 50% to about 60%, from about 1% to about 50%, or about 2% to about 50%, or about 5% to about 50%, or about 10% to about 50%, or about 20% to about 50%, or about 30% to about 50%, or about 40% to about 50% by weight is denatured.

[0024] In various embodiments the frozen milk concentrate may comprise at least about 0.1, 0.15, 0.17, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 1.2, 1.4, 1.6, 1.8, 2, 2.2, 2.4 or 2.5 mg of native (undenatured) lactoferrin per gram of total protein, and various ranges may be selected from between any two of these values, for example, from about 0.1 to about 2.5 mg, about 0.15 to about 2.5 mg, about 0.1 to about 2.2 mg, about 0.15 to about 2.2 mg, about 0.1 to about 2 mg, about 0.15 to about 2 mg of native (undenatured) lactoferrin per gram of total protein.

[0025] In various embodiments, the frozen milk concentrate comprises from about 1.0 to about 8.0% w/w ash, or about 1.0 to about 4.0% w/w ash, for example from

about 1.0 to about 7.0%, about 1.0 to about 6.5%, about 1.0 to about 3.8%, or about 1.0 to about 3.6%, or about 1.0 to about 3.4%, or about 1.0 to about 3.2%, or about 1.0 to about 3.0%, about 1.5 to about 4.0%, about 1.5 to about 3.8%, or about 1.5 to about 3.6%, or about 1.5 to about 3.4%, or about 1.5 to about 3.2%, or about 1.5 to about 3.0%, w/w ash, about 2.0 to about 4.0%, about 2.0 to about 3.8%, or about 2.0 to about 3.6%, or about 2.0 to about 3.4%, or about 2.0 to about 3.2%, or about 2.0 to 2024324023

about 3.0% w/w ash.

[0026] In embodiments where the frozen milk concentrate comprises from about 51% to about 78% by weight total milk solids, optionally from about 60% to about 78% total milk solids or at least about 60%, 65% or 70% total milk solids, and the frozen milk concentrate may comprise from about 1.0 to about 8.0% w/w ash, about 1.0 to about 7.0%, about 2 to about 7.0%, about 2.5to about 7.0%, about 3% to about 7% or about 3.5% to about 7%.

[0027] In various embodiments, the frozen milk concentrate may be a frozen milk protein concentrate. In various embodiments the frozen milk protein concentrate comprises from about 1.0 to about 2.0% w/w ash, for example from about 1.0 to about 1.9%, or about 1.0 to about 1.8%, or about 1.0 to about 1.7%, or about 1.1 to about 2.0%, or about 1.1 to about 1.9%, or about 1.1 to about 1.8%, or about 1.1 to about 1.7%, or about 1.2 to about 2.0%, or about 1.2 to about 1.9%, or about 1.2 to about 1.8%, or about 1.2 to about 1.7% w/w ash. In one embodiment, the frozen milk protein concentrate comprises from about 1.22 to about 1.65% w/w ash.

[0028] In various embodiments the frozen milk protein concentrate comprises from about 0.1 to about 30%w/w fat, about 0.1 to about 25% w/w fat, about 0.1 to about 20% w/w fat, about 0.1 to about 15% w/w fat, about 0.1 to about 10% w/w fat, about 0.1 to about 5% w/w fat or about 0.1 to about 2% w/w fat, about 0.1 to about 0.3%w/w fat, for example from about 0.12% to about 0.3%, or about 0.14% to about 0.3%, or about 0.16% to about 0.3% or about 0.18% to about 0.3%, or about 0.1 to about 0.28%w/w fat, or about 0.12% to about 0.28%, or about 0.14% to about 0.28%, or about 0.16% to about 0.28% or about 0.18% to about 0.28% w/w fat. In one embodiment the frozen milk protein concentrate comprises from about 0.19 to about 0.26%w/w fat.

[0029] In various embodiments the frozen milk protein concentrate comprises at least about 10%, 11%, 12%, 13%, 14%, 15% 16% or 17% by weight total protein. In various embodiments the frozen milk protein concentrate comprises from about 12% to

about 28%, about 13% to about 28%, 14.0 to about 28.0%w/w total protein, for example from about 14.0% to about 26.0%, or about 14.0% to about 25.0%, or about 14.0% to about 24.0%, or about 14.0% to about 23.0%, or about 15.0 to about 28.0% w/w total protein, or about 15.0% to about 26.0%, or about 15.0% to about 25.0%, or about 15.0% to about 24.0%, or about 15.0% to about 23.0%, or about 18.0 to about 28.0%w/w total protein, or about 18.0% to about 26.0%, or about 18.0% to about 2024324023

25.0%, or about 18.0% to about 24.0%, or about 18.0% to about 23.0%, or about 21.0 to about 28.0%w/w total protein, or about 21.0% to about 26.0%, or about 21.0% to about 25.0% w/w total protein.

[0030] In one embodiment, the frozen milk protein concentrate comprises 1.65%w/w ash, 0.26%w/w fat, and 22.2%w/w protein.

[0031] In various embodiments, the frozen milk concentrate comprises at least about 51% by weight total milk solids, or at least about 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65% by weight total milk solids.

[0032] In various embodiments, the frozen milk concentrate comprises at from about 51% to about 78% by weight total milk solids.

[0033] In various embodiments, the frozen milk concentrate comprises from about 60% to about 65% by weight total milk solids.

[0034] In various embodiments, from about 34% to about 40%, about 24% to about 90%, about 34% to about 80%, about 34% to about 75%, about 34% to about 70%, about 34% to about 65%, about 34% to about 60%, or about 34% to about 50% by weight of total milk solids-not-fat in the frozen milk concentrate is protein.

[0035] In various embodiments, the frozen milk concentrate comprises less than about 60% by weight carbohydrate, for example less than about 55%, 50%, 45%, 40%, 35% by weight carbohydrate. In various embodiments, the frozen milk concentrate comprises from about 5% to about 60% by weight carbohydrate, for example, from about 10% to about 60%, or about 15% to about 60%, or about 20% to about 60%, or about 5% to about 50%, or about 10% to about 50%, or about 15% to about 50%, or about 20% to about 50%, or about 5% to about 40%, or about 10% to about 40%, or about 15% to about 40%, or about 20% to about 40%, or about 5% to about 30%, or about 10% to about 30%, or about 15% to about 30%, or about 20% to about 30% by weight carbohydrate.

[0036] In various embodiments, following 24 hours storage at a temperature of - 18°C or less, when the frozen milk concentrate is combined with water to provide a sample comprising 12% by weight total solids, and the sample is mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilised liquid milk, the solubilised liquid milk comprises protein particles, wherein the D[3,2] of the protein particles is less than about 2 μm. 2024324023

[0037] In various embodiments, following 24 hours storage at a temperature of - 18°C or less, when the frozen milk concentrate is combined with water to provide a 12% total solids sample; 100 g of sample is mixed for 5 minutes at 50°C with an antifoaming agent in an automatic solubility index mixer; and 50 mL of sample is centrifuged twice for 5 min at 160 g at room temperature to produce a sedimented sample, the sedimented sample comprising less than about 0.5 mL/50 mL of visible sediment.

[0038] In various embodiments, when the frozen milk protein concentrate is mixed with water to provide a 12% total solids sample, and mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilized milk protein concentrate, the solubilized milk protein concentrate comprising protein particles with a mean particle size D(3,2) of less than 0.1 μm, and/or a D(90) of less than about 1 μm. In various embodiments, the solubilized milk protein concentrate comprises protein particles with a mean particle size D(3,2) of less than 0.1 μm, or less than about 0.09 μm, 0.08 μm, 0.07 μm, or 0.06 μm. In various embodiments, the solubilized milk protein concentrate comprises protein particles with a mean particle size D(90) of less than about 1 μm, or less than about 0.9 μm, 0.8 μm, 0.7 μm, 0.6 μm, 0.5 μm, 0.4 μm, or 0.3 μm.

[0039] In various embodiments, the frozen milk concentrate, following 24 hours, 72 hours, 1 week, 2 weeks, 1 month, or 2, 3, 6, 8, 9, 12, 15, 18, 21 or 24 months storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a sample comprising 12% by weight total solids, and the sample is mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilised liquid milk, the solubilised liquid milk comprises protein particles, wherein the D[3,2] of the protein particles is less than about 0.5, 1, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 2.1, 2.2, 2.3, 2.4, 2.5, 3, 3.5, 4 or 5 μm. In some embodiments, the storage time is 6 months and the D[3,2] of the protein particles is less than about 2 μm; the storage time is 12 months and the D[3,2] of the protein particles is less than about 2 μm; the storage time is 18 months and the D[3,2] of the protein particles is less than about 2 μm; or the

storage time is 24 months and the D[3,2] of the protein particles is less than about 2 μm.

[0040] In various embodiments, the frozen milk concentrate, following 24 hours, 72 hours, 1 week, 2 weeks, 1 month, or 2, 3, 6, 8, 9, 12, 15, 18, 21 or 24 months storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a sample comprising 12% by weight total solids, and the sample is 2024324023

mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilised liquid milk, the solubilised liquid milk comprises protein particles, wherein the D[90] of the protein particles is less than about 2, 5, 7, 8, 9, 10, 11, 12, 10, 15 or 20 μm. In some embodiments, the storage time is 3 months and the D[90] of the protein particles is less than about 10 μm; the storage time is 6 months and the D[90] of the protein particles is less than about 10 μm; the storage time is 12 months and the D[90] of the protein particles is less than about 10 μm; the storage time is 18 months and the D[90] of the protein particles is less than about 10 μm; or the storage time is 24 months and the D[90] of the protein particles is less than about 10 μm.

[0041] In various embodiments, the frozen milk concentrate, following 24 hours, 72 hours, 1 week, 2 weeks, 1, month, 2, 3, 6, 8, 9, 12, 15, 18, 21 or 24 months storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a 12% total solids sample; 100 g of sample is mixed for 5 minutes at 50°C with an antifoaming agent in an automatic solubility index mixer; and 50 mL of sample is centrifuged twice for 5 min at 160 g at room temperature to produce a sedimented sample, the sedimented sample comprises less than about 0.25 mL/50 mL, 0.5 mL/50 mL, 0.75 mL/50 mL, 1 mL/50 mL, 1.5 mL/50 mL, or 2 mL/50 mL of visible sediment. In some embodiments, the storage time is 3 months and the sedimented sample comprises less than about 0.5 mL/50 mL, or 2 mL/50 mL of visible sediment; the storage time is 6 months and the sedimented sample comprises less than about 0.5 mL/50 mL, or 2 mL/50 mL of visible sediment; the storage time is 12 months and the sedimented sample comprises less than about 0.5 mL/50 mL, or2 mL/50 mL of visible sediment; the storage time is 18 months and the sedimented sample comprises less than about 0.5 mL/50 mL, or 2 mL/50 mL of visible sediment; the storage time is 24 months and the sedimented sample comprises less than about 0.5 mL/50 mL, or 2 mL/50 mL of visible sediment.

[0042] In various embodiments, the frozen milk concentrate, following 24 hours, 72 hours, 1 week, 2 weeks, 1, month, 2, 3, 6, 8, 9, 12, 15, 18, 21 or 24 months storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with

water to provide a solubilized sample comprising 12% by weight total solids, the D[3,2] particle size of the protein particles in the solubilized sample increases by less than about 50%, or less than about 45%, 40%, 35%, 30%, 25%, 20%. In some embodiments the solubilised sample may be prepared using a method described herein.

[0043] In various embodiments, of the frozen milk concentrate, following 24 hours, 72 hours, 1 week, 2 weeks, 1, month, 2, 3, 6, 8, 9, 12, 15, 18, 21 or 24 months 2024324023

storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a solubilized sample comprising 12% by weight total solids, the D[90] particle size of the protein particles in the solubilized sample increases by less than about 50%, or less than about 45%, 40%, 35%, 30%, 25%, 20%. In some embodiments the solubilised sample may be prepared using a method described herein.

[0044] In various embodiments, following 24 hours, 72 hours, 1 week, 2 weeks, 1, month, 2, 3, 6, 8, 9, 12, 15, 18, 21 or 24 months storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a solubilized sample comprising 12% by weight total solids, the sedimentation of the solubilized sample increases by less than about 50%, or less than about 45%, 40%, 35%, 30%, 25%, or less than about 20%.

[0045] In various embodiments, total protein comprises at least about 10%, 12%, 15%, 17%, 18% or 20% by weight whey protein.

[0046] In various embodiments, the frozen milk concentrate comprises lipid and protein in a weight ratio of from 0.01:1 to 2:1.

[0047] In various embodiments from about 45% to about 90% of total milk solids- not-fat in the frozen milk concentrate is protein.

[0048] In various embodiments, the frozen milk concentrate comprises from about 14% to about 35% w/w total protein, or from about 14% to about 30% w/w total protein, or from about 14% to about 25% w/w total protein, or from about 14% to about 20% w/w total protein, or from about 15% to about 35% w/w total protein, or from about 15% to about 30% w/w total protein, or from about 15% to about 25% w/w total protein, or from about 15% to about 20% w/w total protein, or from about 16% to about 35% w/w total protein, or from about 16% to about 30% w/w total protein, or from about 16% to about 25% w/w total protein, or from about 16% to about 20% w/w total protein, from about 18% to about 35% w/w total protein, or from about 18% to about 30% w/w total protein, or from about 18% to about 25% w/w total protein, or from

about 18% to about 20% w/w total protein, or from about 20% to about 35% w/w total protein, or from about 20% to about 30% w/w total protein, or from about 20% to about 25% w/w total protein, or from about 21% to about 35% w/w total protein, or from about 21% to about 30% w/w total protein, or from about 21% to about 25% w/w total protein, or from about 22% to about 35% w/w total protein, or from about 22% to about 30% w/w total protein, or from about 22% to about 25% w/w total protein. 2024324023

[0049] In various embodiments, the frozen milk concentrate comprises from about 51% to about 85%, about 51% to about 80%, about 52% to about 85%, about 52% to about 80%, about 53% to about 85%, about 53% to about 80%, about 54% to about 85%, about 54% to about 80%, about 55% to about 85%, about 55% to about 80%, about 57% to about 85%, about 57% to about 80%, about 59% to about 85%, about 59% to about 80%, about 60% to about 85%, or about 60% to about 80%, by weight total milk solids. In various embodiments, the frozen milk concentrate comprises from about 51% to about 80% w/w total milk solids, for example from about 51% to about 78%, or from about 51% to about 75%, or from about 51% to about 73%, or from about 51% to about 70%, or from about 52% to about 80% w/w, or from about 52% to about 78%, or from about 52% to about 75%, or from about 52% to about 73%, or from about 52% to about 70%, or from about 53% to about 80% w/w, or from about 53% to about 78%, or from about 53% to about 75%, or from about 53% to about 73%, or from about 53% to about 70%, or from about 55% to about 80% w/w, or from about 55% to about 78%, or from about 55% to about 75%, or from about 55% to about 73%, or from about 55% to about 70% w/w, or from about 56% to about 78%, or from about 56% to about 75%, or from about 56% to about 73%, or from about 56% to about 70% w/w total milk solids.

[0050] In various embodiments, the frozen milk concentrate comprises less than about 20% w/w fat, for example less than about 19% fat, or less than about 18% fat, or less than about 17% fat, or less than about 16%, or less than about 15%, or less than about 14%, or less than about 13%, or less than about 12%, or less than about 11%, or less than about 10% w/w fat, less than about 9%, or less than about 8%, or less than about 7%, or less than about 6%, or less than about 5%, or less than about 4% w/w fat.

[0051] In various embodiments, the frozen milk concentrate has a density of at least about 1115 kg/m3.

[0052] In various embodiments, the frozen milk concentrate comprises from about 34% to about 45% w/w total solids non-fat.

[0053] In various embodiments, the frozen milk concentrate comprises lipid and protein in a weight ratio of from about 0.01:1 to about 2:1, for example from about 0.02:1 to about 2:1, or about 0.05:1 to about 2:1, or about 0.1:1 to about 2:1, or about 0.2:1 to about 2:1, or about 0.5:1 to about 2:1, or about 1:1 to about 2:1, or about 1.2:1 to about 2:1, or about 1.5:1 to about 2:1, or about 0.01:1 to about 1.5:1, or about 0.02:1 to about 1.5:1, or about 0.05:1 to about 1.5:1, or about 0.1:1 to about 1.5:1, or 2024324023

about 0.2:1 to about 1.5:1, or about 0.5:1 to about 1.5:1, or about 1:1 to about 1.5:1, or about 1.2:1 to about 1.5:1, or about 0.01:1 to about 1:1, or about 0.02:1 to about 1:1, or about 0.05:1 to about 1:1, or about 0.1:1 to about 1:1, or about 0.2:1 to about 1:1, or about 0.5:1 to about 1:1.

[0054] In various embodiments, about 45 to about 90% of total solids-not-fat in the frozen milk concentrate is protein, for example from about 45% to about 85%, or about 45% to about 80%, or about 45% to about 75%, or about 45% to about 70%, or about 45% to about 65%, or about 45% to about 60%, or about 50% to about 90%, or 50% to about 85%, or about 50% to about 80%, or about 50% to about 75%, or about 50% to about 70%, or about 50% to about 65%, or about 50% to about 60%, or about 55% to about 90%, or 55% to about 85%, or about 55% to about 80%, or about 55% to about 75%, or about 55% to about 70%.

[0055] In various embodiments, the frozen milk concentrate comprises less than about 10% by weight of non-dairy ingredients, for example, less than about 9%, less than about 8%, less than about 7%, less than about 6%, less than about 5%, less than about 4%, less than about 3%, less than about 2%, less than about 1% w/w non-dairy ingredients. In some embodiments, the frozen milk concentrate comprises no added non- dairy ingredients.

[0056] In various embodiments, the frozen milk concentrate comprises at least about 10%, 15%, 20% by weight water, for example, at least about 25%, 30%, 35%, 40%, 45% by weight water. In various embodiments, the frozen milk concentrate comprises less than about 50% by weight water, for example, less than about 45%, 40%, 35%, 30% by weight water.

[0057] In various embodiments at least a portion of the water is present as ice. In various embodiments at least about 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50% by weight of the total water in the frozen milk concentrate is present as ice.

[0058] In various embodiments, the liquid milk is whole milk or skim milk.

[0059] In various embodiments, step a) comprises indirectly heating the liquid milk, directly heating the liquid milk, or both.

[0060] In various embodiments, step a) comprises heating the liquid milk at a temperature of less than about 85°C for less than about 50 seconds.

[0061] In various embodiments, the evaporation system comprises between two 2024324023

and five falling film effects.

[0062] In various embodiments, the evaporation system comprises

i) a first falling film effect having a boiling temperature of from about 50 to 70°C, preferably from about 60 to about 66°C,

ii) optionally, one, two or three subsequent falling film effects, each effect having a boiling temperature of from about 45°C to about 65°C, preferably from about 50°C to about 62°C, and

iii) a final falling film effect having a boiling temperature of from about 45°C to about 60°C.

[0063] In various embodiments, each falling film effect has a residence time of less than 60 seconds.

[0064] In various embodiments, the evaporation system comprises falling film evaporation followed by thin film evaporation.

[0065] In various embodiments, the evaporation system comprises a thin film evaporator having a boiling temperature of from about 45°C to about 70°C.

[0066] In various embodiments, the process comprises cooling the concentrated milk at a shear rate of at least 10 s-1.

[0067] In various embodiments, the process comprises cooling the concentrated milk in a scraped surface heat exchanger.

[0068] In various embodiments, cooling comprises introducing the concentrated milk into a scraped surface heat exchanger comprising a first barrel with a temperature of about -8°C to 10°C and a second barrel with a temperature of about -10°C to 5.5°C.

[0069] The invention may also be said broadly to consist in the parts, elements and features referred to or indicated in the specification of the application, individually or collectively, in any or all combinations of two or more of said parts, elements or features, and where specific integers are mentioned herein which have known equivalents in the art to which the invention relates, such known equivalents are deemed to be incorporated herein as if individually set forth. 2024324023

[0070] It is intended that reference to a range of numbers disclosed herein (for example, 1 to 10) also incorporates reference to all rational numbers within that range (for example, 1, 1.1, 2, 3, 3.9, 4, 5, 6, 6.5, 7, 8, 9, and 10) and also any range of rational numbers within that range (for example, 2 to 8, 1.5 to 5.5, and 3.1 to 4.7) and, therefore, all sub-ranges of all ranges expressly disclosed herein are hereby expressly disclosed. These are only examples of what is specifically intended and all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be expressly stated in this application in a similar manner.

[0071] In this specification where reference has been made to patent specifications, other external documents, or other sources of information, this is generally for the purpose of providing a context for discussing the features of the invention. Unless specifically stated otherwise, reference to such external documents is not to be construed as an admission that such documents, or such sources of information, in any jurisdiction, are prior art, or form part of the common general knowledge in the art.

[0072] To those skilled in the art to which the invention relates, many changes in construction and widely differing embodiments and applications of the invention will suggest themselves without departing from the scope of the invention as defined in the appended claims. The disclosures and the descriptions herein are purely illustrative and are not intended to be in any sense limiting.

[0073] Although the present invention is broadly as defined above, those persons skilled in the art will appreciate that the invention is not limited thereto and that the invention also includes embodiments of which the following description gives examples.

BRIEF DESCRIPTION OF THE FIGURES

[0074] The present invention will be described with reference to the accompanying figures, in which:

[0075] Figure 1 shows a process flow diagram for the method described herein. 2024324023

DETAILED DESCRIPTION OF THE INVENTION

[0076] The present invention provides frozen milk concentrates having a high total milk solids and/or high total protein concentration and a low degree of whey protein denaturation. Aggregates present in liquid milks prepared by thawing and diluting frozen milk concentrates are known to cause sedimentation, grittiness and other undesirable properties. Such aggregates may not be readily broken down even by the application of moderate shear. The inventor(s) have demonstrated that, when thawed and processed and despite their high total solids and/or protein content, the frozen milk concentrates described herein produce liquid milk products having one or more of the following properties: a stable milk colloidal system, low sedimentation, protein particles that are small in size, an acceptable flavour profile and that may exhibit no undesirable aggregation, gelling and/or grittiness. Importantly, large aggregates present after the concentrates have been thawed and diluted may be readily broken down by standard processing. Favourably, the frozen milk concentrates may retain one or more of the aforementioned features even following prolonged frozen storage. The invention also provides methods for preparing the frozen milk concentrates.

1. Definitions

[0077] The term “frozen milk concentrate” as used herein refers to a liquid milk concentrate or milk protein concentrate (MPC) that has been frozen to a temperature of less than about -10°C, preferably to a temperature less than about -18°C, or to a temperature less than about -30°C. The frozen milk concentrates comprise, consist essentially of, or consist of, water and milk solids. In various embodiments, the frozen milk concentrate comprises at least about 20% by weight water. In various embodiments at least a portion of the water is present as ice. In various embodiments at least about 30% of the total water in the frozen milk concentrate is present as ice.

[0078] The term “milk protein concentrate” (or MPC) refers to a milk protein product in which greater than 55%, preferably greater than 75% of the dry matter is

milk protein and the ratio of casein to whey proteins is approximately that of milk. The term includes milk protein isolates (MPIs) comprising more than about 90% of dry matter as protein. Such concentrates are known in the art.

[0079] The term “shelf-stable” as used herein in relation to frozen milk concentrates that after storage at a temperature less than about -18°C for at least about 24 or 72 hours, 1 or 2 weeks or 1 month, 2 months, 3 months, 6 months, or at least 2024324023

about 9 months, or at least about 12 months, or at least about 15 months, or at least about 18 months, or at least about 24 months, and when thawed and subjected to moderate shear, provide liquid milk products comprising a stable milk colloidal system, and that have one or more of the following properties: an acceptable flavour profile, low sedimentation or exhibit no more than a minimal increase in sedimentation, small particle size or exhibit no more than a minimal increase in particle size, no undesirable aggregation, gelling and/or grittiness.

[0080] The term “milk solids” as used herein refers to all milk-derived solids remaining following the removal of water, and includes, but is not necessarily limited to, milk sugars (such as lactose), ash (minerals), fat (lipid), and protein (including casein and whey protein). For the avoidance of doubt, the term “total milk solids” refers to all milk solids present in the liquid milk, milk concentrate, MPC or frozen milk concentrate after water has been removed.

[0081] The term “stable colloidal dispersion” or “stable colloidal system” refers to a composition comprising solid particles dispersed in a single, continuous liquid phase. For example, preferably the frozen milk concentrates described herein comprise particles of protein and lipid in an aqueous liquid phase. In various embodiments the stable colloidal dispersion or system does not exhibit any observable sedimentation or separation of the components into layers.

[0082] The term “total protein” as used herein refers to the total amount of protein of a milk concentrate, MPC or frozen milk concentrate as determined by determining the total nitrogen content of the composition and then multiplying by 6.38, without subtracting the non-protein nitrogen content. The total protein content of a sample can be determined by the Kjeldahl method as described in ISO 8968-1:2014.

[0083] The term “denaturable whey protein” as used herein refers to the sum of whey proteins capable of being denatured. Heat treatment results in denaturation of bovine serum albumin (BSA), α-lactalbumin, β-lactoglobulin, lactoferrin,

immunoglobulins. In contrast, glycomacropeptide (GMP) and proteose peptone 5 (pp5) are non-denaturable. The term “denaturable whey protein” therefore excludes GMP and pp5. The total denaturable whey protein may be calculated as described herein.

[0084] The term “denatured” as used herein with reference to whey proteins, and specifically β-lactoglobulin or lactoferrin, refers to such proteins being at least partially unfolded from their native state. Certain denaturable whey proteins denature when 2024324023

subjected to heat treatment of a certain temperature and duration.

[0085] The terms “native” refers to protein that has not been denatured. This includes both denaturable and non-denaturable protein.

[0086] The term “whey” as used herein refers to the liquid composition which is left after casein has been removed from milk.

[0087] The term “comprising” as used in this specification and claims means “consisting at least in part of”. When interpreting each statement in this specification and claims that includes the term “comprising”, features other than that or those prefaced by the term may also be present. Related terms such as “comprise”, “comprised” and “comprises” are to be interpreted in the same manner.

[0088] Unless otherwise stated, the singular forms “a,” “an,” and “the” include the plural reference.

[0089] The term “about” as used herein generally refers to a range of numerical values (e.g. ± 5 to 10% of the recited value) that those skilled in the art would consider equivalent to the recited value. Ranges can be expressed herein as from “about” one particular value, and/or to “about” another particular value. When such a range is expressed, the range is inclusive of the recited values.

[0090] Unless indicated otherwise, all percentage values are on a “by weight” or “w/w” basis.

[0091] As used herein the term “and/or” means “and” or “or”, or both.

[0092] As used herein “(s)” following a noun means the plural and/or singular forms of the noun.

[0093] The general chemical and biological terms used, for example, in the formulae herein have their usual meanings.

2. Manufacturing method

[0094] The present invention relates to a process for preparing a frozen milk concentrate, the process comprising

i) heating liquid milk to a temperature of from about 30°C to about 100°C for less than about 60 seconds to provide a heated milk composition, 2024324023

iv) cooling the concentrated milk under shear to a temperature of less than 10°C to provide a cooled milk concentrate, and

v) freezing the cooled milk concentrate to a temperature of less than about -10°C, preferably less than about -18°C, to provide a frozen milk concentrate;

Liquid milk starting material

[0095] The liquid milk may be prepared from fresh or reconstituted liquid milk.

[0096] The liquid milk is mammalian milk. In some embodiments, the liquid milk may be any mammalian milk including but not limited to bovine, sheep, goat, pig, mouse, water buffalo, camel, yak, horse, donkey, llama or human, with bovine milk being a preferred source.

[0097] In various embodiments, the liquid milk is or comprises whole milk, skim milk, buttermilk, cream, lactose slurry, or any combination of any two or more thereof. In various embodiments the liquid milk is or comprises whole milk or skim milk. In various embodiments the liquid milk is whole milk or skim milk.

[0098] In various embodiments, the liquid milk may be prepared by blending skim milk, whole milk, cream, lactose-rich slurries, or any combination of any two or more thereof to achieve a desired composition of protein, lipid and/or lactose. Various methods for standardization are well known in the art, such as those described in the Dairy Processing Handbook (Bylund, G. (Ed.) 1995 Tetra Pak Processing Systems AB, S-221 86 Lund, Sweden). In one embodiment, the liquid milk is prepared according to CODEX CXS 2024324023

207-1999.

[0099] In various embodiments, the whole milk may comprise about 14% by weight total solids, about 3.6% by weight protein, about 3.8% by weight fat, and about 6.5% by weight lactose. In one embodiment whole milk may be standardized to provide a weight ratio of protein to solids non-fat of about 3.5:10 and a weight ratio of fat to total solids ratio of about 2.7:10. In various embodiments, the whole milk may be standardized to provide a weight ratio of protein to solids non-fat ratio of from about 3.5:10 to about 4.5:10.

[00100] In various embodiments the skim milk may comprise about 10.2% by weight total solids, about 3.6% by weight protein, about 0.1% by weight fat, and about 6.5% by weight lactose. In one embodiment skim milk may be standardized to provide a weight ratio of protein to solids non-fat of about 3.5:10 and a weight ratio of fat to total solids ratio of about 0.01:10. In various embodiments, the skim milk may be standardized to provide a weight ratio of protein to solids non-fat ratio of from about 3.5:10 to about 4.5:10.

[00101] In various embodiments the liquid milk may be pasteurized. Any standard methods known in the art may be used, for example, holding liquid milk at a temperature of about 72°C for approximately 15 seconds.

[00102] In various embodiments, the liquid milk may be subjected to treatment to hydrolyse saccharides in the milk, such as lactose. In some embodiments, the liquid milk may be subjected to treatment with a hydrolytic enzyme, such as β-galactosidase. β- galactosidase catalyses the hydrolysis of the β-glycosidic bond between galactose and other sugars to produce galactooligosaccharides (GOS).

Pre-heating

[00103] The inventor(s) have found that when liquid milk is subjected to a low- medium heat thermal profile throughout the preheating/evaporation and concentrate handling process, certain undesirable changes associated with preparing concentrates

with high total milk solids and/or protein content may be minimised such as alterations to protein structure and age-thickening of the concentrate. Despite the moderate heat treatment, effective heat transfer is achieved and the resulting high total solids/total protein frozen milk concentrates have one or more of the favourable properties described herein.

[00104] The process may comprise heating the liquid milk to a temperature of from 2024324023

about 30°C to about 100°C for less than about 240, 180, 150, 120, or 60 seconds to provide a heated milk composition.

[00105] In various embodiments, the process may comprise heating the liquid milk to a temperature of at least about 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95,or at least about 100°C for less than about 240, 210, 180, 150, 120, 90, 60, 55, 50, 45, 40, 35, 30, 25, 20, 15 seconds, and any ranges may be selected from between any two or these values, for example, from about 30°C to about 100°C, from about 30°C to about 90°C, from about 30°C to about 80°C, from about 30°C to about 70°C, from about 30°C to about 60°C, from about 30°C to about 50°C, from about 40°C to about 100°C, from about 40°C to about 90°C, from about 40°C to about 80°C, from about 40°C to about 70°C, from about 40°C to about 60°C, from about 50°C to about 100°C, from about 50°C to about 90°C, from about 50°C to about 80°C, from about 50°C to about 70°C for less than about240, 210, 180, 150, 120, 90, 60, 55, 50, 45, 40, 35, 30, 25, 20, 15 seconds.

[00106] In various embodiments, the process comprises heating the liquid milk to a temperature of less than about 100°C, or less than about 95, 90, 85, 80, 75, 70°C for less than about 240, 210, 180, 150, 120, 90, 60, 50, 40, or 30 seconds. In a preferred embodiment, the process comprises heating the liquid milk to a temperature of less than about 85°C for less than about 50 seconds.

[00107] In various embodiments the process may comprise indirect heating, direct heating, or a combination thereof. In various embodiments, step a) comprises indirectly heating the liquid milk, directly heating the liquid milk, or both. In various embodiments, indirect heating may comprise heating using a plate heat exchanger. In various embodiments, direct heating may comprise heating using direct steam injection (DSI). The preheating arrangement may also be built in to commercial milk evaporators. Milk is heated indirectly over a number of stages up to 60-70°C followed by either indirectly or directly in a number of stages to 73-120°C or directly from 60 to 150°C. The milk is then held for 10 – 300 s before flashing down in stages to the first effect boiling temperature

(Refstrup, Proceedings of 25th International Dairy Congress, 1998). Other examples of indirect and direct heating are known in the art and will be readily apparent to those skilled in the art.

[00108] In various embodiments, the process may comprise indirectly heating the liquid milk to a temperature of at least about 50°C over a period of at least about 30 seconds and/or directly heating the liquid milk (or indirectly heated milk) at a 2024324023

temperature of at least about 70°C for at least about 20 seconds. In various embodiments, the process comprises indirectly heating the liquid milk to a temperature of at least about 65°C over a period of at least about 30 seconds and/or directly heating the liquid milk (or indirectly heated milk) at a temperature of at least about 80°C for at least about 30 seconds. In various embodiments, the process comprises indirectly heating the liquid milk to a temperature of at least about 50°C, or at least about 55°C, or at least about 60°C, or least about 65°C. In various embodiments, the process comprises indirectly heating the liquid milk to a temperature of about 50°C to about 150°C, or at least about 50°C to about 100°C, or at least about 50°C to about 80°C. In various embodiments, the process comprises indirectly heating the liquid milk to a temperature of about 50°C to about 150°C for about 30 seconds to about 300 seconds. In various embodiments, the process comprises indirectly heating the liquid milk to a temperature of about 50°C to about 150°C for about 30 seconds to about 90 seconds.

[00109] In various embodiments, the process may comprise directly heating the liquid milk (or the indirectly heated milk) at a temperature of at least about 70°C for at least about 20 seconds.

[00110] In various embodiments, the process may comprise indirectly heating the liquid milk at a temperature of

i) from about 73°C to about 80°C for less than about 240 seconds,

ii) from about 80°C to about 85°C for less than about 50 seconds,

iii) from about 85°C to about 90°C for less than about 5 seconds,

[00111] In various embodiments, the process may comprise directly heating the liquid milk (or the indirectly heated milk) at a temperature of

i) from about 73°C to about 80°C for less than about 240 seconds,

ii) from about 80°C to about 85°C for less than about 75 seconds,

iii) from about 85°C to about 90°C for less than about 20 seconds,

iv) from about 90°C to about 95°C for less than about 20 seconds,

v) from about 95°C to about 100°C for less than about 20 seconds.

[00112] In various embodiments, the process may comprise directly heating the 2024324023

liquid milk (or the indirectly heated milk) at a temperature of

i) from about 73°C to about 80°C for less than about 240 seconds,

ii) from about 80°C to about 85°C for less than about 60 seconds,

iii) from about 85°C to about 90°C for less than about 15 seconds,

iv) from about 90°C to about 95°C for less than about 15 seconds,

v) from about 95°C to about 100°C for less than about 15 seconds.

[00113] In a preferred embodiment, the process may comprise heating the liquid milk at a temperature of less than about 85°C for less than about 50 seconds.

[00114] Advantageously, heating used to provide the frozen milk concentrates of the present invention is typically lower than used for powdered whole milk concentrates, meaning the process is more energy efficient.

Concentration

[00115] To reach the high total solids of the frozen milk concentrates of the present invention, concentration may be achieved using a falling film evaporator and/or a thin film evaporator.

[00116] Accordingly, the process for preparing a frozen milk concentrate comprises providing an evaporation system that comprises a falling film evaporator and removing moisture from the heated milk composition through evaporative processing using the evaporation system to produce a concentrated milk comprising at least about 51% total milk solids.

[00117] In various embodiments, the heated milk may be heated during concentration to a temperature of about 40°C to about 90°C, or about 40°C to about 80°C, or about 40°C to about 70°C, or about 50°C to about 90°C, or about 50°C to

about 80°C, or about 50°C to about 70°C, or about 60°C to about 90°C, or about 60°C to about 80°C. In a preferred embodiment, the heated milk may be heated during concentration to a temperature of about 40°C to about 70°C.

[00118] In various embodiments, the evaporation system may be operated at a temperature of at least about 40°C, or at least about 45°C, or at least about 50°C. In various embodiments, the evaporation system may be operated at a temperature of less 2024324023

than about 90°C, or less than about 85°C, or less than about 80°C, or less than about 75°C, or less than about 70°C.

[00119] In various embodiments, the evaporation system may be operated at a temperature of from about 40°C to about 90°C, or about 40°C to about 80°C, or about 40°C to about 70°C, or about 45°C to about 90°C, or about 45°C to about 80°C, or about 55°C to about 70°C, or about 50°C to about 90°C, or about 50°C to about 80°C, or about 50°C to about 70°C, or about 55°C to about 90°C, or about 55°C to about 80°C, or about 55°C to about 70°C, or about 60°C to about 90°C, or about 60°C to about 80°C.

[00120] In various embodiments, the evaporation system may be operated at a shear rate of at least about 10 s-1.

[00121] The evaporation system may comprise a falling film evaporator. In various embodiments, the evaporation system may comprise a thin film evaporator. In various embodiments, the evaporation system may comprise a falling film evaporator, and a thin film evaporator, preferably, a falling film evaporator followed by a thin film evaporator.

[00122] Falling film evaporators comprise vertical tubes in which a fluid is concentrated as it progresses downwards. In falling film evaporators, the liquid product stream flows down the internal walls of a large number of thin wall tubes. Falling film evaporators typically have up to 9 effects operating at different boiling temperatures. The product flows downward in up to 13 passes across these effects, for example, a Mechanical Vapour Re-compressor (MVR) effect can have up to 8 passes. Typical whole milk evaporators operate at boiling temperatures between 75°C to 45°C (preferably 65°C to 50°C). The first effect is normally operated at the highest temperature and final concentration is done between 50-56°C. The temperature difference is averaged across the number of effects. In various embodiments, the falling film evaporator may have multiple effects at different temperatures and/or pressures. In various embodiments, the evaporation system comprises a falling film evaporator having multiple effects with a

sequentially lowering temperature profile. In various embodiments, the evaporation system comprises a falling film evaporator having multiple effects with boiling temperatures of 60°C, 56°C and 54°C respectively and steam side temperatures of 66°C, 61°C, and 58°C respectively. In various embodiments, the feed rate is 250 kg/h. In the context of the present invention, a falling film evaporator may be used to produce a frozen milk concentrate with up to 60% total milk solids. 2024324023

[00123] Thin film evaporators are also known as wiped film evaporators. Thin film evaporators comprise a cylindrical heated body and a rotor. In the context of the present invention, a thin film evaporator may be used to produce a frozen milk concentrate comprising more than about 60% total milk solids.

[00124] In a typical embodiment, the heated milk undergoes evaporation in a thin film evaporator with a jacket pressure of 86 kPa, a steam jacket temperature of 95°C, a boiling pressure of 20 kPa, a boiling temperature of 60°C, and a rotor speed of 350 rpm. In various embodiments, the heated milk undergoes evaporation in a thin film evaporator with a jacket pressure of about 75 to about 90 kPa. In various embodiments, the heated milk undergoes evaporation in a thin film evaporator with a steam jacket temperature of about 92 to about 97°C. In various embodiments, the heated milk undergoes evaporation in a thin film evaporator with a boiling pressure of from about 10 to about 30 kPa. In various embodiments, the heated milk undergoes evaporation in a thin film evaporator with a boiling temperature of from about 45 to about 70°C. In various embodiments the evaporation system comprises a thin film evaporator with boiling temperatures of from about 30°C to about 75°C, preferably from about 55 to about 65°C.

[00125] In various embodiments, the evaporation system comprises at least two, three, or four effects that comprises a falling film evaporator and/or a thin film evaporator. In various embodiments, the heated milk is concentrated using an evaporation system comprising at least two, three, or four effects that comprises a falling film evaporator. In various embodiments, the heated milk is concentrated using an evaporation system comprising two, three, or four effects. In various embodiments, the evaporation system comprises between two and five falling film effects.

[00126] In various embodiments the evaporation system comprises from 1 to 9 falling film effects operating at sequentially lowering boiling temperatures from about 75°C to about 45°C, preferably from about 65 to about 50°C.

[00127] In various embodiments, the evaporation system may comprise at least one, two, three, four or five falling film effects. In various embodiments the evaporation system may comprise between one and five, between two and five, between three and five, between one and four, between two and four, three or four, between three and five or four or five falling film effects.

[00128] In various embodiments, the heated milk is concentrated using an 2024324023

evaporation system comprising at least two, three, or four evaporators connected in series that comprises a falling film evaporator and/or a thin film evaporator. In various embodiments, the heated milk is concentrated using an evaporation system comprising at least two, three, or four evaporators connected in series or parallel that comprises a thin film evaporator. In various embodiments, the heated milk is concentrated using an evaporation system comprising at least two, three, or four evaporators connected in series.

[00129] In various embodiments, the heated milk is concentrated using an evaporation system comprising a falling film evaporator and a thin film evaporator. In various embodiments, the heated milk is concentrated using an evaporation system comprising at least two, three, or four effects that comprises a falling film evaporator and a thin film evaporator.

[00130] In various embodiments, the evaporation system comprises a falling film evaporator followed by thin film evaporator.

[00131] In various embodiments, the evaporation system comprises

[00132] The heated milk is concentrated in the evaporation system to produce a concentrated milk comprising at least about 51% total milk solids, for example, at least about 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%,

65%. In various embodiments, the heated milk is concentrated to produce a concentrated milk comprising from about 51% to about 80%, about 52% to about 80%, about 53% to about 80%, about 54% to about 80%, about 55% to about 80%, about 56% to about 80%, about 57% to about 80%, about 58% to about 80%, about 59% to about 80%, or about 60% to about 80% total milk solids. In various embodiments, the heated milk is concentrated to produce a concentrated milk comprising from about 51% 2024324023

to about 78% total milk solids.

[00133] In various embodiments, the milk is not heated above 70°C for longer than 60 minutes, or longer than 33 minutes at any time during the process. In various embodiments, the milk is not heated above 80°C for longer than 300 seconds at any time during the process.

[00134] In various embodiments, the temperatures used during the process provide a frozen milk concentrate having a low degree of whey protein denaturation. In various embodiments, the temperatures used during the process provide a frozen milk concentrate wherein less than about 40% by weight of β-lactoglobulin in the frozen milk concentrate is denatured.

Cooling and freezing

[00135] Following concentration, the concentrated milk is cooled. The process comprises cooling the concentrated under shear to a temperature of less than about 10°C to provide a cooled milk concentrate.

[00136] Any suitable equipment for achieving cooling under these conditions that is known in the art may be used. In various embodiments, the process comprises cooling the concentrated milk in a scraped surface heat exchanger (SSHE). In various embodiments, the process comprises cooling comprises introducing the concentrated milk into a scraped surface heat exchanger comprising a first barrel with a temperature of about -4°C and a second barrel with a temperature of about -5.5°C.

[00137] In various embodiments, the process comprises cooling the concentrated milk at a shear rate of at least about 10 s-1. In various embodiments, the process comprises cooling the concentrated milk with shear rates of from about 10 s-1 to about 50 s-1.

[00138] The process comprises freezing the cooled milk concentrate to a temperature of less than about -10°C, preferably less than about -18°C, to provide a

frozen milk concentrate. In various embodiments, the process comprises freezing the cooled milk concentrate to a temperature of less than about -10°C, -12°C, -14°C, -15°C ,-16°C ,-18°C, -20°C, -25°C , or -30°C. In various embodiments, the process comprises freezing the cooled milk concentrate to a temperature of between about -10°C and about -80°C, or about -15°C to about -80°C, or about -18°C to about -80°C, or about -20°C to about -80°C, or about -25°C to about -80°C, or about -30°C to about -80°C, or about - 2024324023

10°C and about -40°C, or about -15°C to about -40°C, or about -18°C to about -40°C, or about -20°C to about -40°C, or about -25°C to about -40°C, or about -30°C to about - 40°C, or about -10°C and about -30°C, or about -15°C to about -30°C, or about -18°C to about -30°C, or about -20°C to about -30°C.

[00139] In various embodiments the cooled concentrated milk may be frozen in slabs in a vertical plate freezer. In various embodiments, the cooled concentrated milk is frozen at a freezing rate of at least 1 μm s-1. In various embodiments, the process comprises freezing the cooled milk concentrate into slabs, sheets, or blocks.

[00140] In various embodiments the concentrated milk undergoes no homogenization prior to freezing.

Milk protein concentrates

[00141] In another aspect, the invention provides a process comprising

wherein the evaporation system is operated at a temperature of from about 40°C to about 70°C; and optionally with a shear rate of at least about 10 s-1. 2024324023

[00142] Generally, MPCs are prepared by processes invoking ultrafiltration to prepare a stream enriched in casein and whey protein. In another embodiment, the milk protein concentrate may be prepared by blending a stream of skim milk with a stream of whey protein concentrate, optionally treating either the skim milk stream or the combined stream by cation exchange Suitable MPCs for use herein may be prepared from a mixture of MPCs.

[00143] The milk protein may be provided in the form of a calcium depleted MPC. Calcium-depleted MPCs are MPCs in which the calcium content is lower than the corresponding non-depleted MPC. These products generally also have a lower content of other divalent cations, for example, magnesium, than corresponding non-depleted products.

[00144] MPCs for use in the invention may have calcium that is manipulated by a cation exchange method. The manufacture and application of these calcium-depleted MPCs have been previously disclosed in US Patent 7,157,108, published PCT application WO2008/026940 and US published patent application 2010/0021595. These documents are fully incorporated herein by reference. Other methods of preparing calcium depleted MPCs will be apparent to a skilled worker.

[00145] In various embodiments, the milk protein concentrate starting material may be prepared by subjecting whole or skim milk to ultrafiltration (UF) and collecting the UF retentate or subjecting whole or skim milk to microfiltration (MF) and collecting the MF permeate. Ultrafiltration may be performed with diafiltration (DF). UF and or MF may be performed under conditions sufficient to produce a milk protein concentrate comprising at least about 15% by weight total solids and at least about 12% by weight total protein.

[00146] In various embodiments the MPC may comprise at least about 15% by weight total solids, or at least about 16%, or at least about 17%, or at least about 18%, or at least about 19%, or at least about 20% by weight total solids. In various

embodiments, the MPC may comprise from about 15% to about 65% by weight total solids, or from about 20% to about 65% by weight total solids, for example from about 15% to about 30%, or about 15% to about 25%, or about 15% to about 20%, or about 16% to about 30%, or about 16% to about 25%, or about 16% to about 20%, or about 17% to about 30%, or about 17% to about 25%, or about 17% to about 20%, or about 18% to about 30%, or about 18% to about 25%, or about 20% to about 30%, or about 2024324023

20% to about 25% by weight total solids.

[00147] In various embodiments the MPC may comprise at least about 12% by weight total protein, or at least about 12.5%, or at least about 13%, or at least about 13.5%, or at least about 14%, or at least about 14.5%, or at least about 15% by weight total protein. In various embodiments, the MPC may comprise from about 12% to about 35% total protein, for example from about 12% to about 30%, or about 12% to about 25%, or about 12% to about 20%, from about 13% to about 30%, or about 13% to about 25%, or about 13% to about 20%, from about 14% to about 30%, or about 14% to about 25%, or about 14% to about 20%, from about 15% to about 30%, or about 15% to about 25%, or about 15% to about 20%, or about 16% to about 30%, or about 16% to about 25%, or about 16% to about 20%, or about 17% to about 30%, or about 17% to about 25%, or about 17% to about 20%, or about 18% to about 30%, or about 18% to about 25%, or about 20% to about 30%, or about 20% to about 25% by weight total solids.

[00148] The process comprises heating the MPC to a temperature of from about 30°C to about 100°C for less than about 60 seconds to provide a heated MPC. The hearing may be direct or indirect heating, performed under conditions and using equipment as to described above.

[00149] In various embodiments, the process may comprise indirectly heating the MPC at a temperature of

i) from about 55°C to about 65°C for less than about 50 seconds,

ii) from about 65°C to about 75°C for less than about 15 seconds,

to provide a heated MPC.

[00150] In various embodiments, the process may comprise directly heating the MPC (or the indirectly heated MPC) at a temperature of

i) from about 55°C to about 65°C for less than about 50 seconds,

ii) from about 65°C to about 75°C for less than about 15 seconds,

to provide a heated MPC.

[00151] The process further comprises removing moisture from the heated MPC 2024324023

through evaporative processing using the evaporation system to produce a concentrated milk comprising at least about 14% by weight total protein and at least about 20% by weight total solids.

[00152] The evaporative processing may comprise falling film and/or thin film evaporation. In various embodiments, the evaporation system comprises a falling film evaporator and/or a thin film evaporator. In various embodiments, the evaporation system comprises a falling film evaporator and a thin film evaporator. In various embodiments, the evaporation system comprises a falling film evaporator. In various embodiments, the evaporation system comprises a thin film evaporator.

[00153] Suitable equipment and operating conditions are described above.

[00154] The concentrated milk may be cooled and frozen as described above.

3. Frozen milk concentrates

[00155] The present invention provides a frozen milk concentrate having a total milk solids content greater than 51% by weight and/or a total protein content greater than 12% by weight. Casein present in frozen milk concentrates is known to be subject to cryodestabilisation, whereby casein particles aggregate to form large protein aggregates that are not readily broken down after the concentrate is thawed and diluted in water. The size of the aggregates and the degree of instability increases as the total milk solids content of a frozen milk concentrate increases, which has previously limited the production of frozen milk concentrates to a total solids content of less than 50%. Surprisingly, using the methods described herein, the present inventor(s) have prepared frozen milk concentrates having a high total solids and/or protein content that comprise protein aggregates that are readily broken down upon thawing and dilution in water and the application of moderate shear. Furthermore, the resulting milk product maintains a fresh milk flavour. The frozen milk concentrates described herein may have less and delayed aggregation and low sedimentation after storage for longer periods of time.

[00156] Without wishing to be bound by any theory, the inventor believes that the methods described herein promote the formation of non-covalent bonding between casein molecules (rather than covalent bonding), which is more readily broken down upon thawing and dilution in water when a moderate degree of shear is applied.

[00157] Total solids can be measured using any method known to skilled worker, such as Test Method NZTM 3.12.15, which enables measurement of total milk solids in a 2024324023

frozen product. When the total milk solids is greater than 55%, samples for total solids measurements may be diluted straight after collection (to avoid lactose crystallization and/or gelation which may affect analysis accuracy) with water at a temperature of 60°C using 4 parts water to 1 part sample by weight and stirred for 2 mins with a magnetic stirrer. The diluted samples can then be tested using NZTM 3.12.15 and the result multiplied by 5 to obtain total solids content of the sample.

[00158] In various embodiments, the frozen milk concentrate comprises at least about 4% w/w lactose, or at least about 5%, 10%, 15%, 20% w/w lactose. In various embodiments, the frozen milk concentrate comprises from about 4% to about 60% by weight lactose, for example, from about 5% to about 60%, about 10% to about 60%, or about 15% to about 60%, or about 20% to about 60%, or about 4% to about 50%, or about 5% to about 50%, or about 10% to about 50%, or about 15% to about 50%, or about 20% to about 50%, or about 4% to about 40%, or about 5% to about 40%, or about 10% to about 40%, or about 15% to about 40%, or about 20% to about 40%, or about 4% to about 30%, or about 5% to about 30%, or about 10% to about 30%, or about 15% to about 30%, or about 20% to about 30% by weight lactose.

Denaturation

[00159] The inventor(s) have found that high total solids and/or protein in frozen milk concentrates with favourable properties may be achieved when there is a low degree of whey protein denaturation. Whey protein includes glycomacropeptide (GMP) and proteose peptone 5 (pp5), which are casein-related proteins as well as denaturable whey proteins including bovine serum albumin (BSA), α-lactalbumin, β-lactoglobulin, lactoferrin, and immunoglobulins. Heat treatment can cause denaturation of these denaturable whey proteins. Whey protein denaturation can be measured, as can denaturation of individual whey protein such as β-lactoglobulin and lactoferrin. Methods for measuring the denaturation of whey proteins are known to a skilled worker. Examples are also described herein.

[00160] The frozen milk concentrates described herein have a low degree of whey protein denaturation. In various embodiments, less than about 40% by weight of denaturable whey protein in the frozen milk concentrate is denatured. In particular, the frozen milk concentrates have a low degree of β-lactoglobulin denaturation. In particular, less than about 40% by weight of β-lactoglobulin in the frozen milk concentrate is denatured. 2024324023

[00161] In one aspect, the invention provides a frozen milk concentrate comprising from about 14% to about 35% by weight total protein and at least about 20% by weight total milk solids, wherein the total protein comprises β-lactoglobulin of which less than about 40% by weight is denatured.

[00162] In another aspect the invention provides a frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein total protein in the frozen milk concentrate comprises β-lactoglobulin of which less than about 40% by weight is denatured.

[00163] Thermal denaturation of whey protein and/or any other thermally sensitive milk protein such as lactoferrin, and/or whey protein nitrogen index (WPNI) can be measured to indicate low heat treatment. Methods for measuring whey protein denaturation, including β-lactoglobulin and lactoferrin denaturation are known in the art. β-lactoglobulin denaturation may be measured using the procedure described in Elgar et al., Journal of Chromatography A, 878 (2000) 183–196 according to Test Method 3 described herein.

[00164] In various embodiments, the frozen milk concentrate may comprise β- lactoglobulin of which less than about 40%, 39%, 38%, 37%, 36%, 35%, 34%, 33%, 32%, 31%, 30%, 28%, 26%, 25%, 24%, 23%, 22%, 21%, 20%, 19%, 18%, 17%, 16%, 15%, 12%, 10% by weight is denatured.

[00165] In various embodiments, the frozen milk concentrate may comprise denaturable whey protein of which less than about 40%, 39%, 38%, 37%, 36%, 35%, 34%, 33%, 32%, 31%, 30%, 28%, 26%, 25%, 24%, 23%, 22%, 21%, 20%, 19%, 18%, 17%, 16%, 15%, 12%, 10% by weight is denatured.

[00166] In various embodiments the total protein comprises lactoferrin of which less than 95% by weight is denatured, for example less than about 90%, 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%, 45%, 40%, 35%, 30%, 25%, 20%, 15%, 10%, or less than about 5% by weight is denatured. Preferably, the total protein comprises

lactoferrin of which less than 50% by weight is denatured, for example less than about 49%, 48%, 47%, 46%, 45%, 44%, 43%, 42%, 41%, or less than about 40% by weight is denatured.

[00167] In general, the amount of lactoferrin that is denatured in the frozen milk concentrates of the present invention is more similar to the amount of denatured lactoferrin in fresh milk than to the amount in whole milk powder. 2024324023

[00168] In various embodiments the frozen milk concentrate may comprise at least about 0.1, 0.15, 0.17, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 1.2, 1.4, 1.6, 1.8, 2, 2.2, 2.4 or 2.5 mg of native (undenatured) lactoferrin per gram of total protein, and various ranges may be selected from between any two of these values, for example, from about 0.1 to about 2.5 mg, about 0.15 to about 2.5 mg, about 0.1 to about 2.2 mg, about 0.15 to about 2.2 mg, about 0.1 to about 2 mg, about 0.15 to about 2 mg of native (undenatured) lactoferrin per gram of total protein.

[00169] The degree of lactoferrin denaturation in the frozen milk concentrates described herein may be measured using methods known in the art. For example, lactoferrin denaturation may be measured by HPLC according to the method described in Indyk et al., 2007, Food Chemistry 101, pp 838-844, or the by method described in Test method 3a.

[00170] If a sample collected before denaturation is available (i.e. a sample of the milk composition prior to the pre-heating and concentration), the Test method 3 described herein in the Examples may be used to measure β-lactoglobulin denaturation.

[00171] When a pre-denaturation sample is not available, the degree of whey protein denaturation can be estimated using the following method:

i) If necessary, the sample is reconstituted at 3% protein in 0.1M NaCl. The sample is then split into three fractions.

i. For Fraction 1, the total crude protein is measured using the Kjeldahl method as total nitrogen × 6.38. This measurement includes casein, denatured whey protein aggregates, and soluble undenatured whey protein.

ii. Fraction 2 is centrifuged at 7,000 × g for 20 minutes without adjusting the pH. This step removes the whey protein aggregates,

while the soluble undenatured whey protein and casein stay in solution. The supernatant is collected and the protein content measured, again using the Kjeldahl method as total nitrogen × 6.38. This measurement includes casein and soluble undenatured whey protein.

iii. Fraction 3 is acidified to pH 4.6 with 15% acetic acid, recording the 2024324023

added volume to correct for the dilution caused. The fraction is again centrifuged at 7,000 × g for 20 minutes. This step removes the casein and whey protein aggregates, while the soluble undenatured protein stays in solution. The supernatant is collected and the protein content measured, again using the Kjeldahl method as total nitrogen × 6.38, and adjusting to account for the dilution caused by the addition of acetic acid. This measurement includes just the soluble undenatured whey protein.

ii) The casein content can be calculated as fraction 2 − fraction 3; the denatured whey protein aggregate content can be calculated as fraction 1 – fraction 2; and the total whey protein content can be calculated as (fraction 1 – fraction 2) + fraction 3.

iii) The soluble protein fraction can be characterised by testing the fractions 1 and 3 by HPLC to eludicate what protein sources may have been blended.

iv) The percent whey protein denaturation can then be calculated using the following formula:

𝑑𝑒𝑛𝑎𝑡𝑢𝑟𝑒𝑑 𝑤ℎ𝑒𝑦 𝑝𝑟𝑜𝑡𝑒𝑖𝑛 𝑎𝑔𝑔𝑟𝑒𝑔𝑎𝑡𝑒𝑠 % 𝑤ℎ𝑒𝑦 𝑝𝑟𝑜𝑡𝑒𝑖𝑛 𝑑𝑒𝑛𝑎𝑡𝑢𝑟𝑎𝑡𝑖𝑜𝑛 = × 100 𝑡𝑜𝑡𝑎𝑙 𝑤ℎ𝑒𝑦 𝑝𝑟𝑜𝑡𝑒𝑖𝑛

[00172] Whey protein nitrogen index (WPNI) is a measure of whey protein solubility and is expressed as the amount of whey protein nitrogen that is water soluble relative to the total amount of protein nitrogen present. Higher heat exposure causes whey proteins to denature and become less water soluble, resulting in a low WPNI value. Lower heat exposure means less heat exposure and less whey protein denaturation giving a higher WPNI value. In various embodiments, the frozen milk concentrate has a WPNI of at least about 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, or 10. Preferably, the frozen milk concentrate has a WPNI of from about 4 to about 10, about 4 to about 9, about 4 to about 8, about 5 to about 10, about 5 to about 9 or about 5 to

about 8; most preferably, about 5 to about 8. Methods for measuring the WPNI will be known to a skilled worker.

[00173] Preferably, frozen milk concentrates may be stored at a temperature of less than about -10°C, preferably less than about -18°C. In embodiments, for example, when little shear will be applied to the frozen milk concentrate after dilution, the frozen milk concentrates is preferably stored at a temperature of less than about -25°C. In 2024324023

various embodiments fluctuation in temperature during storage is restricted, preferably to less than about +/- 1°C, more preferably less than about +/- 0.5°C.

Properties and uses

[00174] The frozen milk concentrates of the present invention resolubilize in water to provide a product similar to fresh liquid milk and that exhibits minimal protein aggregation. In various embodiments, the frozen milk concentrate resolubilizes in water. Solubility of frozen milk concentrates can be determined by measuring the protein particle size profile and/or sedimentation levels after re-solubilisation. Exemplary methods for measuring these parameters are described in the examples section. Other methods are well known in the art and will be apparent to the skilled worker.

[00175] The protein particles present in the milk concentrate described herein when solubilised comprise a large proportion of particles having a small particle size. Larger particles of insoluble protein, in particular particles >3 μm, are often less desirable as they can lead to an unpleasant gritty or sandy mouthfeel in certain applications. Larger particles can also be prone to sedimentation. Particle size distribution (PSD) is indicative of low levels of aggregated proteins in liquid milk produced by thawing and dilution of the frozen concentrates described herein. Particle sizes are reported as the surface weighted mean diameter (D[3,2]) and the value at which 90% of particles have a lower diameter (D(90)). Particle size distribution (PSD) may be measured according to Test method 1 described in the Examples. As would be understood by a skilled worker, the PSD measurement of the samples will also include measurement of the fat particles. However, these particles are not expected to significantly change in size, therefore any differences seen in PSD can be attributed to protein particles.

[00176] In various embodiments, when the frozen milk concentrate is mixed with water to provide a 12% total solids sample, and mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilized liquid milk, the solubilized liquid milk comprises a stable colloidal dispersion comprising protein particles with a mean

particle size D(3,2) of less than 2 μm, and/or a D(90) of less than about 10 μm. In various embodiments, when the frozen milk concentrate is mixed with water to provide a 12% total solids sample, and mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilized liquid milk, the solubilized liquid milk comprises protein particles with a mean particle size D(3,2) of less than 2 μm, and/or a D(90) of less than about 10 μm. In various embodiments, the solubilized liquid milk comprises protein 2024324023

particles with a mean particle size D(3,2) of less than 2 μm, or less than about 1.9 μm, 1.8 μm, 1.7 μm, 1.6 μm, or 1.5 μm. In various embodiments, the solubilized liquid milk comprises protein particles with a mean particle size D(90) of less than about 10 μm, or less than about 9.5 μm, 9 μm, 8.5 μm, 8 μm, 7.5 μm, 7 μm, 6.5 μm, or 6 μm.

[00177] In one aspect, the invention provides a frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein following 24 hours storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a sample comprising 12% by weight total solids, and the sample is mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilised liquid milk, the solubilised liquid milk comprises protein particles, wherein the D[3,2] of the protein particles is less than about 2 μm.

[00178] In one aspect, the invention provides a frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein, following 24 hours storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a 12% total solids sample; 100 g of sample is mixed for 5 minutes at 50°C with an antifoaming agent in an automatic solubility index mixer; and 50 mL of sample is centrifuged twice for 5 min at 160 g at room temperature to produce a sedimented sample, the sedimented sample comprises less than about 0.5 mL/50 mL of visible sediment.

[00179] In various embodiments, the frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein following 3 months, 6 months, 12 months, 18 months, or 24 months storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a sample comprising 12% by weight total solids, and the sample is mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilised liquid milk, the solubilised liquid milk comprises protein particles, wherein the D[3,2] of the protein particles is less than about 2 μm.

[00180] In various embodiments, the frozen milk concentrate comprising at least about 51% by weight total milk solids, wherein, following 3 months, 6 months, 12

months, 18 months, or 24 months storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a 12% total solids sample; 100 g of sample is mixed for 5 minutes at 50°C with an antifoaming agent in an automatic solubility index mixer; and 50 mL of sample is centrifuged twice for 5 min at 160 g at room temperature to produce a sedimented sample, the sedimented sample comprises less than about 0.5 mL/50 mL of visible sediment. 2024324023

[00181] In various embodiments, the solubilized liquid milk is homogenized to form a homogenized solubilized liquid milk, the homogenized solubilized liquid milk comprises protein particles with a mean particle size D(3,2) of less than 1 μm.

[00182] Sedimentation levels are indicative of the aggregated protein strengths and thus the stability over shelf life of the concentrates. Sedimentation may be measured according to Test method 2. In various embodiments, the frozen milk concentrate is mixed with water to provide a 12% total solids sample; 100 g of sample is mixed for 5 minutes at 50°C with an antifoaming agent in an automatic solubility index mixer; and 50 mL of sample is centrifuged twice for 5 min at 160 g at room temperature to produce a sedimented sample, the sedimented sample comprising less than about 0.5 mL/50 mL of visible sediment, or less than about 0.4 mL, or less than about 0.3 mL or less than about 0.2 mL, or preferably less than about 0.1 mL/50 mL of visible sediment.

[00183] In various embodiments, the frozen milk concentrate has a G’ of at least about 5000 Pa when thawed. G’ can be measured using an Anton Paar Rheometer.

[00184] The frozen slabs of frozen milk concentrate of the present invention are able to be cut into small pieces for use in food service applications due to the ice structure formed.

[00185] In various embodiments, the frozen milk concentrate is shelf-stable at - 18°C for at least about 3 months, or at least about 6 months, or at least about 9 months, or at least about 12 months, or at least about 15 months, or at least about 18 months, or at least about 24 months.

[00186] The inventor has found that by applying the methods of the invention described herein the liquid milk produced by thawing and dilution of the frozen milk concentrates retains the fresh flavour of milk, for example, the fresh flavour of New Zealand milk. In various embodiments, the frozen milk concentrate has a protein profile similar to that of fresh milk. For example, in various embodiments the weight ratio of casein and whey in the frozen milk concentrate is similar to that of fresh milk.

[00187] In a preferred embodiment, liquid whole milk prepared from frozen milk concentrates of the present invention may comprise 3.4% fat, 3.3% protein, 4.8% lactose, and 12% total solids. Liquid whole milk prepared from frozen milk concentrates of the present invention may subsequently be used to make a range of dairy products, such as butter, buttermilks, cheese and byproducts, creams, casein, yoghurt, icecream, desserts, bubble tea, barista milk, evaporated milk, and sweetened condensed milk. 2024324023

[00188] The following non-limiting examples are provided to illustrate the present invention and in no way limit the scope thereof.

EXAMPLES

Test method 1 – Overhead stirring test

[00189] The overhead stirring test is performed to determine the particle size distribution of a frozen milk concentrate.

[00190] The test method is as follows:

1. Weigh out required quantity of frozen concentrate to provide 12% total solids in a 500 g sample in a 115 mm diameter stainless steel or glass container.

2. Start the water bath and set the temperature to 55°C.

3. Add warm water (55°C) to the container and make-up the volume to 500 g ± 0.1 g and place it in a water bath at 55°C.

4. Allow to mix using an 60 mm diameter Rushton turbine over-head stirrer placed 20 mm from the base of the stainless steel for 30 minutes at 400 rpm.

5. Sample the mixed solution and measure particle size distribution using the Malvern Mastersizer 3000. The setting on the Malvern includes refractive indices of 1.4 and 1.33 for the particles and water respectively.

Test method 2 – Sedimentation

[00191] This test is carried out to determine insolubility by measuring sedimentation levels in a test sample.

[00192] The target total solid content in the test samples is 12%.

[00193] The test method is as follows:

1. Calculate the quantity of the frozen concentrate required for 100 mL of 12% total solid reconstituted milk. 2024324023

2. Set water bath temperature to 50 ± 0.2°C.

3. Place a bottle of reverse osmosis (RO) water and mixing jar in the water bath.

4. Put the mixing jar on a scale and weigh the concentrate in it.

[00194] Use warm RO water to make 100 mL.

5. Add 2-3 drops of silicone antifoam to the mixing jar.

6. Mix the solution for 5 min using the Solindex (Glen Charles, Auckland, New Zealand) mixer.

7. Remove the jar from the Solindex mixer and stand in water bath for 10min (add 1 or 2 drops of antifoam if foam is present).

[00195] Transfer the 100 mL solution into 2 x 50 mL centrifuge tubes.

[00196] Centrifuge at 160 g, 20°C for 5 min.

8. Discard the top layer of fatty material from the tube. Siphon to the 10 mL mark, take care not to disturb the sediment level.

9. If sediment level is above 10 mL discontinue procedure at this stage and record results as >10 mL.

[00197] Top up to 50 mL with warm water. Centrifuge again at 160 g, 20°C for 5 min.

10. Read against a strong light holding the tube vertically at eye level and record the sediment level.

Test method 3 - β-lactoglobulin denaturation

[00198] The method used herein relies on HPLC (Elgar et al (2000) J Chromatography A, 878, 183-196). The HPLC system was a Waters e2695 Alliance Separation Module interfaced with a 2489 UV/Vis detector. Two samples are used — one sample of the concentrated milk or MPC to be tested (the “test” sample), and one sample of the milk prior to the pre-heating and concentration (the “original” sample). 2024324023

[00199] Step 1: remove casein and insoluble whey protein aggregates. The pH of both samples is reduced to 4.6 to precipitate the caseins. The samples are then centrifuged to remove the precipitated caseins and the insoluble whey protein aggregates.

[00200] Step 2: reverse phase HPLC. The residual soluble denaturable β- lactoglobulin in the test sample is determined using reversed phase HPLC (Elgar et al., 2000) as and can be expressed as grams protein/100 grams total solids.

[00201] The total soluble denaturable β-lactoglobulin in the undenatured sample is determined by the same method, using the original sample from Step 1.

Step 3: calculate % denatured β-lactoglobulin. First, the values for residual soluble denaturable β-lactoglobulin and total soluble denaturable β-lactoglobulin are normalised using the total solids content of the two samples prior to step 1. The total amount of denatured β-lactoglobulin as a percentage of the total amount of denaturable β- lactoglobulin can then be calculated by subtracting the total amount of denaturable β- lactoglobulin with the residual soluble denaturable present in the sample. The following formula gives the percentage (%) of denatured β-lactoglobulin in the sample.

𝑟𝑒𝑠𝑖𝑑𝑢𝑎𝑙 𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑑𝑒𝑛𝑎𝑡𝑢𝑟𝑎𝑏𝑙𝑒 𝛽 − 𝑙𝑎𝑐𝑡𝑜𝑔𝑙𝑜𝑏𝑢𝑙𝑖𝑛⁄%𝑇𝑆 𝑜𝑓 "𝑡𝑒𝑠𝑡" 𝑠𝑎𝑚𝑝𝑙𝑒 1− × 100 𝑡𝑜𝑡𝑎𝑙 𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑑𝑒𝑛𝑎𝑡𝑢𝑟𝑎𝑏𝑙𝑒 𝛽 − 𝑙𝑎𝑐𝑡𝑜𝑔𝑙𝑜𝑏𝑢𝑙𝑖𝑛 ⁄%𝑇𝑆 𝑜𝑓 "𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙" 𝑠𝑎𝑚𝑝𝑙𝑒

Test method 3a - Lactoferrin denaturation

[00202] The method used herein relies on HPLC (Elgar et al (2000) J Chromatography A, 878, 183-196). The HPLC system was a Waters e2695 Alliance Separation Module interfaced with a 2489 UV/Vis detector. Two samples are used — one sample of the concentrated milk or MPC to be tested (the “test” sample), and one sample of the milk prior to the pre-heating and concentration (the “original” sample).

[00203] Step 1: remove casein and insoluble whey protein aggregates. The pH of both samples is reduced to 4.6 to precipitate the caseins. The samples are then

centrifuged to remove the precipitated caseins and the insoluble whey protein aggregates.

[00204] Step 2: reverse phase HPLC. The residual lactoferrin in the test sample is determined using reversed phase HPLC (Elgar et al., 2000) as and can be expressed as grams protein/100 grams total solids. 2024324023

[00205] The total lactoferrin in the undenatured sample is determined by the same method, using the original sample from Step 1.

[00206] Step 3: calculate % denatured lactoferrin. First, the values for residual lactoferrin and total lactoferrin are normalised using the total solids content of the two samples prior to step 1. The total amount of denatured lactoferrin as a percentage of the total amount of denaturable lactoferrin can then be calculated by subtracting the total amount of denaturable lactoferrin with the residual soluble denaturable present in the sample.

The following formula gives the percentage (%) of denatured lactoferrin in the sample.

𝑟𝑒𝑠𝑖𝑑𝑢𝑎𝑙 𝑙𝑎𝑐𝑡𝑜𝑓𝑒𝑟𝑟𝑖𝑛 ⁄%𝑇𝑆 𝑜𝑓 "𝑡𝑒𝑠𝑡" 𝑠𝑎𝑚𝑝𝑙𝑒 1− × 100 𝑡𝑜𝑡𝑎𝑙 𝑙𝑎𝑐𝑡𝑜𝑓𝑒𝑟𝑟𝑖𝑛 ⁄%𝑇𝑆 𝑜𝑓 "𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙" 𝑠𝑎𝑚𝑝𝑙𝑒

Test method 4 – Method of preparing samples for sensory evaluation.

[00207] This method is to ensure the consistency of samples prepared for sensory evaluation and especially avoid the introduction of any off-flavours or textures. This method was used from the 6-month timepoint onwards of the sensory shelf-life study of frozen whole milk concentrate (FWMC) prototypes.

[00208] The test sample is a single strength milk, and the target total solid content is 12.5%.

[00209] The test protocol is as follows:

[00210] Step 1: Cut blocks.

1. Do not thaw or temper blocks before cutting.

2. Cut the blocks into sizeable pieces and vacuum pack approximately 500 g per bag. Discard vacuum sealed product 1 week after cutting.

[00211] Step 2: Make single strength milk.

[00212] A Thermomix blender is recommended to be used in preparing the single strength milk.

[00213] The sample preparation is as follows:

1. Determine the amount of frozen concentrate required based on application to be used in. 2024324023

2. Take out required number of vacuum-packed blocks. Do not thaw the block.

3. Add the required amount of FWMC to Thermomix bowl.

4. Add the required amount of RO water at 60°C to the bowl.

5. Transfer the bowl to the Thermomix. Set the temperature to 60°C and run at speed 0.5 until the blade turns freely without knocking and the temperature reaches 60°C.

6. Gradually increase the speed to 2.5 and set the timer for 5 minutes.

7. While the FWMC is mixing, run hot water through the homogeniser. Adjust the pressures to 30-40 bar second stage while leaving the first stage released. Prepare an ice bath.

8. When the 5 minutes is complete, pass the milk through the homogeniser. Adjust the homogeniser pressure to 50 bar second stage, then 200 bar total, collect into the stainless-steel beaker. Rinse the homogeniser thoroughly with hot water. If more batches of product are to be homogenised, continue running hot water through the homogeniser. Allow the product to run until it reaches the correct consistency before collecting product. If no more product is to be homogenised, release the second stage pressure, then the first stage and switch off the homogeniser.

9. Rinse the Thermomix bowl with hot water and drain it.

10. Pour the homogenised milk back into the Thermomix bowl. Check that the total solids and adjust to accordingly to 12.5%.

11. Heat to 75°C, at speed 2.5 and set timer for 1 minute.

12. Rinse the stainless-steel beaker with hot water and drain.

13. When the 1 minute is complete, pour the milk into the stainless-steel beaker and place in the ice bath. Rinse the Thermomix bowl with hot water.

14. Cool the milk in the ice bath to 20°C while stirring with the spoon.

15. Pack and store the milk in fridge till ready to use.

16. Discard any remaining frozen blocks that has not been used by the end of the day.

Test method 5 – Formal Sensory Panel Evaluation

[00214] This formal sensory panel evaluation method documents the formal sensory panel assessment of frozen whole milk concentrates.

[00215] The samples assessed by the panel were prepared using Test Method 4. 2024324023

[00216] The sensory assessment protocol is as follows:

i) All samples were evaluated by trained sensory panel B (n=8-13) utilising a sensory lexicon created during the initial attribute generation session (see Table A).

ii) For each timepoint, one attribute generation and training session, and two- four training, and calibration sessions were held prior to two hybridised descriptive analysis evaluation sessions.

iii) The number of training and calibration, and evaluation sessions varied due to the number of samples included in that timepoint evaluation.

iv) For each evaluation, samples were duplicated within a session and duplicated, triplicated, or quadruplicated across two sessions to check panellist reproducibility.

v) The samples were presented to the panellists in a balanced and randomised order.

vi) Sensory attributes were related to aroma, taste, flavour, and texture. All attributes were assessed on 150 mm line scales.

vii) Definitions of each attribute are presented in Table 1. All attributes were anchored from “Absent” to “Intense”, except Thickness which was anchored from “Thin” to “Thick”.

viii) The samples were tasted under red lights (to mask any differences in appearance) at ambient temperature (~20 °C) in small, clear plastic cups labelled with random 3-digit codes.

ix) The sensory data was collected on tablets using Compusense Cloud®

Version 24.0.26799 2024/04/03. Panellist attribute intensity scores were

checked, charted, and analysed in Minitab® version 20.4 to ensure consistency across panellists and across duplicated samples.

x) Sample duplicate intensity scores were combined, and panellist mean intensity scores for each attribute were calculated before conducting General Linear Modelling (GLM) through Analysis of Variance (ANOVA). 2024324023

xi) For attributes with significance between samples, Tukey’s Pairwise Comparison with significance set at p<0.05 % was used to define means separation.

Table A: Sensory attributes and definitions.

Attribute Definition Cooked Milk Aroma The aroma associated with heat treatment of milk. Sweet The basic taste associated with sugar (sucrose). Salt The basic taste associated with table salt. Creamy The flavour associated with New Zealand fresh cream. Cooked Milk The flavour associated with heat treatment of milk. Cowy * The flavours associated with clean animals and their environment, cow’s breath. Lactone * The flavours reminiscent of a dishcloth that was used to wipe up spilt milk and left damp overnight. Also described as musty or apricot yoghurt. Stale/Tallow * The off-flavour associated with oxidised fat. From not fresh, fridgy, lightstruck, stale, tallow rancid and fishy.

Thickness The thickness of the samples as perceived in the mouth. Mouthcoating The amount of product/ fat film left in the mouth from the sample directly after swallowing/spitting sample. Astringency Sensation causing drying up of saliva and puckering of the cheeks. Baked The flavour associated with cooked sugars. Biscuit * (added at 14-month timepoint) * These attributes were not included in the sensory evaluation of Example 6 trial samples (Samples I, O, and P) but were included in the sensory evaluation of Example 7 trial samples (Samples E, R, K, S, J, and U).

Example 1

[00217] All samples were prepared using standardised whole milk. Pasteurised cream, pasteurised skim milk, and a 20% total solids lactose slurry were combined and standardised to produce a standardised whole milk comprising a 0.35 ratio of protein/solids non-fat and a 0.27 ratio of fat/total solids. The standardised whole milk comprised 14% total solids, 3.6% protein, 3.8% fat, and 6.5% lactose. 2024324023

Sample D

[00218] A frozen whole milk concentrate comprising 55% by weight total solids was prepared as follows.

[00219] Standardised whole milk was subjected to the following pre-heating: indirect heating by plate heat exchanger to a temperature of 65°C followed by direct steam injection at 80°C for 30 seconds.

[00220] The pre-heated milk was introduced into a NZDRI Research Evaporator which is a type of falling film evaporator and concentrated at sequential boiling temperatures of 60°C, 56°C, and 54°C in the first, second and third effects, respectively, with a residence time of less than 1 minute per effect to a total solids content of 55% by weight. The table below lists the NZDRI Research Evaporator tube details.

Table 1: Evaporator tube details

Calandria Number of Tubes Tube Internal Diameter (mm) Tube Length (m) First 4 48 15 Second 2 48 15 Third 1 48 15

[00221] The concentrated milk was cooled in a scraped surface heat exchanger at - 4°C in the first barrel then -5.5°C in the second barrel, both barrels have at least 10 s-1 shear rate.

[00222] The cooled concentrated milk was frozen overnight in three formats (sheets or cubes and blocks) to -18°C with a freezing rate of at least 1 μm s-1.

Sample E

[00223] A frozen whole milk concentrate comprising 60% by weight total solids was prepared as follows.

[00224] Standardised whole milk was subjected to the following pre-heating: indirect heating by plate heat exchanger to a temperature of 65°C followed by direct 2024324023

steam injection at 80°C for 30 seconds.

[00225] The pre-heated milk was introduced into a falling film evaporator and concentrated at sequential boiling temperatures of 60°C, 56°C and 54°C in the first, second and third effects, respectively, with a residence time of less than 1 minute per effect. The concentrated milk was further concentrated in a thin-film evaporator (Artisan Industries horizontal unit with 12” diameter rotor within a 12.25” diameter housing with a 0.5 m2 heat transfer surface) with a jacket pressure of 80 kPa absolute, a steam jacket temperature of 93°C, boiling pressure of 20 kPa absolute, boiling temperature of 60°C, feed rate of 200 kg/h and a rotor speed of 300 rpm to a total solids content of 60% by weight.

[00226] The concentrated milk was cooled and stored as described above for Sample D.

Sample F

[00227] A frozen whole milk concentrate comprising 60% by weight total solids was prepared as follows.

[00228] Standardised whole milk was subjected to the following pre-heating: indirect heating by plate heat exchanger to a temperature of 65°C followed by direct steam injection at 88°C for 30 seconds.

[00229] The pre-heated milk was introduced into a falling film evaporator and concentrated at sequential boiling temperatures of 60°C, 56°C and 54°C in the first, second and third effects, respectively, with a residence time of less than 1 minute per effect. The concentrated milk was further concentrated in a thin-film evaporator with a jacket pressure of 80 kPa absolute, a steam jacket temperature of 93°C, boiling pressure of 20 kPa absolute, boiling temperature of 60°C, feed rate of 200 kg/h and a rotor speed of 300 rpm to a total solids content of 60% by weight.

[00230] The concentrated milk was cooled and stored as described above for Sample D.

Sample G

[00231] A frozen whole milk concentrate comprising 68% by weight total solids was prepared as follows. 2024324023

[00232] Standardised whole milk was subjected to the following pre-heating: indirect heating by plate heat exchanger to a temperature of 65°C followed by direct steam injection at 80°C for 30 seconds.

[00233] The pre-heated milk was introduced into a falling film evaporator and concentrated at sequential boiling temperatures of 60°C, 56°C and 54°C in the first, second and third effects, respectively, with a residence time of less than 1 minute per effect. The concentrated milk was further concentrated in a thin-film evaporator) with a jacket pressure of 86 kPa absolute, a steam jacket temperature of 95°C, boiling pressure of 20 kPa absolute, boiling temperature of 60°C, feed rate of 150 kg/h and a rotor speed of 300 rpm to a total solids content of 68% by weight.

[00234] The concentrated milk was cooled and stored as described above for Sample D.

Sample H – MPC

[00235] A frozen whole milk protein concentrate (MPC) comprising 22% by weight total protein was prepared as follows.

[00236] MPC concentrate was prepared by fractionating fresh, pasteurised skim milk (4.56 g/100 g protein, 0.09 g/100 g fat) using a 4 stage, continuous ultrafiltration (UF) plant equipped with 5 kDa UF membranes. The UF processing continued until a retentate was produced comprising approximately 14% by weight total protein. The retentate was diluted with demineralised water and further ultra-filtered (diafiltration or DF). The UF and DF processing temperature was constantly held at 10°C. UF/DF was continued until a total solids content of approximately 17 g/100 g and a total protein content of approximately 14 g/100 g was achieved.

[00237] The resulting UF retentate was preheated to 60°C using a plate heat exchanger followed by direct steam injection heating at 70°C for 10 seconds before it was evaporated through an evaporator up to 23 g/100 g total solids. The milk protein

concentrate was concentrated in a thin-film evaporator with a jacket pressure of 130 kPa absolute, boiling pressure of 20 kPa absolute, boiling temperature of 60°C and a rotor speed of 600 rpm. The concentrated MPC was then cooled by scraped surface heat exchange at 5°C. The cooled concentrated milk protein concentrate was frozen overnight in sheets or cubes or blocks to -18°C with a freezing rate of 1 µm s-1 to provide a frozen milk protein concentrate. 2024324023

Example 1a

Samples I-U

[00238] Frozen whole milk concentrates were prepared analogously to sample E with the following variations:

[00239] Standardised whole milk was subjected to the following pre-heating: indirect heating by plate heat exchanger to a temperature of 65°C followed by direct steam injection at the specified temperature in table 1a for 30 seconds.

[00240] The pre-heated milk was introduced into a falling film evaporator and concentrated at sequential boiling temperatures as specified in table 1a in the first, second and third effects, respectively, with a residence time of less than 1 minute per effect. The concentrated milk was further concentrated in a thin-film evaporator with a jacket pressure as specified, a steam jacket temperature as specified, boiling pressure of 20 kPa absolute, boiling temperature of 60°C, feed rate as specified and a rotor speed as specified to a total solids content as specified in table 1a.

[00241] Sample I to S were prepared using standardised whole milk. Pasteurised cream, pasteurised skim milk, and a 20% total solids lactose slurry were combined and standardised to produce a standardised whole milk comprising a 0.35 ratio of protein/solids non-fat and a 0.27 ratio of fat/total solids. The standardised whole milk comprised 14% total solids, 3.6% protein, 3.8% fat, and 6.5% lactose.

[00242] Samples T and U were prepared using standardised whole milk. Pasteurised cream, pasteurised skim milk, and a 20% total solids lactose slurry were combined and standardised to produce a standardised whole milk comprising a 0.38 ratio of protein/solids non-fat and a 0.27 ratio of fat/total solids. The standardised whole milk comprised 14% total solids, 3.6% protein, 3.8% fat, and 6.8% lactose.

Table 1a:

Sampl Total Direct Falling film Jacket Steam Fee Roto e solids steam evaporator pressur jacket d r content injectio temperature e, temperatur rate spee , by n s absolute e d weight 2024324023

I 60% 80°C 60°C, 60°C, 83 kPa 94°C 150 355 55°C kg/h rpm J 60% 80°C 60°C, 56°C, 86 kPa 95°C 150 356 54°C kg/h rpm K 60% 80°C 64°C, 60°C, 80 kPa 93°C 200 300 kg/h rpm 55°C L 66% 80°C 60°C, 56°C, 80 kPa 93°C 150 355 54°C kg/h rpm M 68% 80°C 60°C, 56°C, 80 kPa 93°C 150 355 54°C kg/h rpm N 66% 80°C 67°C, 63°C, 83 kPa 94°C 150 355 58°C kg/h rpm O 60% 100°C 61°C, 59°C, 88 kPa 96°C 150 355 54°C kg/h rpm P 60% 120°C 62°C, 60°C, 85k Pa 95°C 145 355 54°C kg/h rpm Q 60% 80°C 76°C, 74°C, 81 kPa 94°C 155 355 72°C kg/h rpm R 60% 90°C 64°C, 61°C, 80 kPa 93°C 200 300 56°C kg/h rpm S 60% 80°C 64°C, 60°C, 80 kPa 93°C 200 300 55°C kg/h rpm T 62% 80°C 60°C, 56°C, 80 kPa 95°C 155 355 54°C kg/h rpm U 60% 80°C 60°C, 56°C, 80 kPa 95°C 155 356 54°C kg/h rpm Example 2

[00243] The composition of the samples is indicated in Table 2.

Table 2: Composition of samples

Samples Ash Fat g/100g Lactose Protein g/100g g/100g g/100g D 2.73 14.5 23.2 14.2 E 2.73 15.1 29.1 15.2 2024324023

F 2.73 15.1 29.1 15.2 G 3.13 19.0 32.0 17.0 H 1.65 0.26 - 22.0

Example 2a

[00244] The composition of the samples is indicated in Table 2a.

Table 2a: Composition of samples

Samples Ash g/100g Fat g/100g Lactose g/100g Protein g/100g I 3.00 16.0 29.2 14.9 J 3.11 11.7 25.3 15.9 K 2.72 14.8 27.8 14.7 L 3.05 9.5 32.3 16.8 M 3.18 7.2 31.4 17.1 N 3.14 18.1 36.7 15.2 O 2.90 15.8 28.6 14.9 P 3.00 15.8 28.0 14.9 Q 3.00 16.1 29.4 15.3 R 2.68 15.2 27.6 14.8 S 2.57 13.5 - 15.1 U 3.24 14.8 23.0 16.5 Example 3

[00245] The particle size distribution of the samples was measured using Test method 1. Samples were measured between 3 - 4 months after preparation. The results are presented in Table 3.

Table 3: Particle size distribution of samples.

Samples D(3,2) μm D(90) μm

D 1.48 8.87 E 1.61 7.82 F 1.16 5.60 G 1.80 6.31 H 0.05 0.20 2024324023

Example 3a

[00246] The particle size distribution of the samples was measured using Test method 1, except the water temperature and water bath were 60°C and the stirring was done at 100 rpm for 10 min then 350 rpm for 30 min. Samples were measured 3 - 4 months after preparation. The results are presented in Table 3a.

Table 3a: Particle size distribution of samples.

Samples D(3,2) μm D(90) μm I 0.992 3.35 J 0.92 3.19 K 1.02 6.4 L 0.6 4.85 M 0.524 1.68 O 0.935 2.95 P 0.912 2.68 Q 0.981 3.37 R 1.16 5.57 S 1.13 6.01 T 0.959 2.9 U 0.96 3.4 Example 4

[00247] Sedimentation levels after storage at -18°C were measured using Test method 2. The results are presented in Table 4.

Table 4: Sedimentation in samples following storage.

Sample Age of Sediment tube 1 Sediment tube Average samples (mL/50mL) 2 (mL/50mL) sediment

(mL/50mL) D 18 months 0.10 0.12 0.11 E 10 months <0.1 <0.1 <0.1 F 3 months 0.5 0.5 0.5 G 18 months 0.1 0.12 0.11 H 24 months <0.1 <0.1 <0.1 2024324023

Example 4a

[00248] Sedimentation levels after storage at -18°C were measured using Test method 2. The results are presented in Table 4a.

Table 4a: Sedimentation in samples following storage.

Sample Age of Sediment tube 1 Sediment tube Average samples (mL/50mL) 2 (mL/50mL) sediment (mL/50mL) I 5 months 0 0 0 J 0.75 months 0 0 0 K 1 month 0.1 0.1 0.1 L 1 month 0.8 0.9 0.85 M 1 month 0.15 0.2 0.175 O 5 months <0.1 <0.1 <0.1 P 5 months 4 4.5 4.25 Q 5 months 0.1 0.1 0.1 R 1 month 0.2 0.2 0.2 T 5 months 0 0 0 U 0.75 months 0 0 0 S 3 months 0 0 0

Example 5

[00249] β-lactoglobulin denaturation was measured according to Test method 3. The results are presented in Table 5.

Table 5: Level of β-lactoglobulin denaturation in samples

Samples β-Lactoglobulin β-Lactoglobulin (g/L) denaturation (%) Fresh milk 3.249 0 D 9.831 14.3% E 11.414 12.4% 2024324023

F 8.38 35.7%

G 12.459 12.2%

H 13.495 5.0%

Whole milk powder manufactured 1.18 g/L 54.3% at Fonterra Pahiatua, batch number 23182628 (WMP reconstituted to 13% solids) Example 5a

[00250] β-lactoglobulin and lactoferrin denaturation was measured according to Test methods 3 and 3a. The results are presented in Tables 6 and 6a.

Table 6: Level of β-lactoglobulin denaturation in samples

Samples β-Lactoglobulin (g/L) β-Lactoglobulin denaturation (%) Fresh milk 3.41 0.00 I 12.04 14.13% J 12.78 13.00% K 11.41 11.95% O 6.25 57.84% P 2.62 83.22% Q 12.42 11.47% R 7.94 37.75% T 13.41 14.79% U 13.34 10.51%

Table 6a – Lactoferrin measurements in serum phase (Method 3a) on feed and concentrates and %denatured lactoferrin

Lactoferrin mg/L % Lactoferrin Samples Feed Concentrate Denatured 37% 2024324023

I 0.116 0.073 T 0.127 0.088 31% O 0.119 0.028 76% P 0.110 0.017 85%

Example 6: Sensory results

[00251] Samples were prepared according to Test Method 4 and were evaluated as white milks. Sensory evaluation was completed using Test Method 5 where the results are specific to just this one-off evaluation of Samples I, O and P (Example 1). Sample I was significantly lower in cooked milk aroma, cooked milk flavour, and astringency while significantly higher in sweet taste, than Sample O and Sample P. The hypothesis was proven where Sample O and Sample P are more cooked (aroma and flavour) than Sample I. Sample P was significantly more astringent than the other two samples.

Table 7: Mean intensity scores given by trained panellists for sensory attributes of FWMC samples on a 150 mm scale (0 - absent; 150 - highly intense) for Sample I, Sample O, and Sample P. Threshold level is 20 mm.

Sample I O P Cooked Milk Aroma 40 73 73 Sweet 68 61 61 Salt 44 45 46 Creamy 63 63 63 Cooked Milk 51 63 63 Thickness 65 66 65 Mouthcoating 61 64 62 Astringency 66 69 75

Example 7: Shelf-life study for FWMC

[00252] For the sensory shelf-life study, samples at 12.5% total solids were prepared according to Test Method 4 and evaluated as white milks. When commercial samples were included for the study, the liquid commercial samples were poured straight into the sample cups while the powder format were recombined by adding 25 g in 200 mL room temperature water to make the 12.5% total solids sample. 2024324023

Sensory evaluation was completed using Test Method 5 where the results cover Examples 1, and 2 and are presented in Table 8. All the FWMC samples (Samples E, R, K, S, J, and U) are significantly lower in cooked milk flavour than the UHT Blue Milk across all timepoints (Table 8). Sample E was significantly less cooked than WMP (20 °C) across all timepoints. This is the only sample comparison with WMP (20 °C) due to being the only sample evaluated across all timepoints. The intensity of cooked milk flavour for the FWMC samples is at or below weak while the intensity of the UHT Blue Milk is approaching moderate. All samples were evaluated using the full sensory lexicon (Table 2 in Test Method 5), but only cooked milk flavour is shown in Table 8 for reporting purposes.

Table 8: Mean intensity scores given by trained panellists for cooked milk flavour of FWMC samples on a 150 mm scale (0 - absent; 150 - highly intense) per timepoint. Threshold level is 20 mm.

Time points (months) 0 0.75 1 3 4 6 8 9 12 14 18 Sample E 43 40 38 32 30 28 30 Sample R 31 Sample K 36 32 31 Sample S 32 29 28 Sample J 41 Sample U 27 36 WMP (-18˚C) 46 50 53 47 46 44 46 37 WMP (20˚C) 42 45 Pasteurised Blue Top Milk 0 0 0 6 0 0 0 0 0 UHT Blue Milk 65 62 60 59 65 63 63 59

Example 8: 3% Protein Chilled Yoghurt

[00253] The following examples describe the production of yoghurt from a frozen milk concentrate according to the invention and compares the properties and sensory attributes of the yoghurts to that of yoghurts prepared from fresh milk and whole milk powder. 2024324023

[00254] The samples were made into yoghurt as follows:

1. Weigh out required quantity of fresh milk or whole milk powder or frozen milk concentrates to provide approximately 3% protein in a 20kg sample. 2. Weigh out required non-dairy ingredients. 3. Start the water bath and set the temperature to 55°C. 4. Add warm water (55°C) to the container and make-up the volume to 20 ± 0.1 kg. and place it in a water bath at 55°C. 5. Allow to mix using an over-head stirrer placed 20 mm from the base of the stainless steel for 30 minutes at 400 rpm. 6. The recombined samples were then homogenized using Rannie Homogenizer (Denmark) which was set to 2-stage homogenizing pressure; 1st stage at 150 bar and 2nd stage at 50 bar. 7. The homogenized samples were heat treated at 95°C for 5 minutes using a plate- heat exchanger. 8. The samples then cooled down to 42°C. 9. The samples were inoculated with starter culture and let fermented until at least a pH of 4.6 was reached. 10. Yoghurts were cooled down to 20°C and smoothed using back pressure valve at 1 bar. 11. Yoghurts were packed for functionality, sensory and shelf-life testing.

[00255] Method of analysis

1. The pH of the yoghurts was measured post-fermentation after cooling the samples to 20°C and stirring the samples to break the gel structure. The pH of the samples was measured by equilibrating samples to 20°C and measuring using a pH probe (EC620132, Thermo Scientific) after calibrating using standards at pH 4, 7, and 10 (Pronalys, LabServ). 2. The appearance of the samples was assessed by using a spoon to scoop the yoghurt and a qualitative assessment of the textural properties from the point of the consumer was made. 3. The fracture force and firmness of the yoghurts was measured using a TA-TX2 texture analyzer. 4. Viscosity was measured using a Haake VT 500 Viscometer with coaxial cylinder geometry. The sample was poured into the cup to the fill line and placed into the rheometer ensuring the sample was tempered to 10°C before the measurement was started. The sample was subjected to a pre-shear of 300 s-1 for 1 minute followed by a rest period of 1 minute prior to measurement. The sample is subjected to a shear rate sweep from 0.001 – 398 s-1 with the viscosity taken at 50 s-1.

[00256] The results are shown in Table 9.

Table 9: Properties comparison between 3% Protein Chilled Yoghurt made from fresh milk, whole milk concentrates

Properties Yoghurt from fresh Yoghurt from whole Yoghurt from frozen milk milk powder milk concentrates 2024324023

pH post- 4.41 4.52 4.42 fermentation Texture: Fracture 20 20 27 force (g) Texture: Firmness 430 403 570 (g mm) Viscosity at 50 s-1 720 860 825 (mPa s) Appearances at Day Smooth, Soft Smooth, Soft Smooth, Soft 7 Appearances at Day Smooth, Soft Smooth, Soft Smooth, Soft 42

Example 9: 3% Protein Ambient Yoghurt

[00257] The following examples describe the production of yoghurt from a frozen milk concentrate according to the invention and compares the properties and sensory attributes of the yoghurts to that of yoghurts prepared from fresh milk and whole milk powder.

[00258] Samples were prepared similar to Example 8 with one additional step prior to packing.

1. Samples were prepared according to Example 1: 3% Protein Chilled Yoghurt steps I – X. 2. Yoghurts were given another heat treatment at 75°C for 30 seconds. 3. Yoghurts were packed for functionality, sensory and shelf-life testing.

[00259] Analysis was done similar to the methods described in Example 8.

[00260] The results are shown in Table 10.

Table 10: Properties comparison between 3%Protein Ambient Yoghurt made from fresh milk, whole milk powder and frozen milk concentrates.

Properties Yoghurt from fresh Yoghurt from whole Yoghurt from frozen milk milk powder milk concentrates pH post- 4.05 4.12 4.08 fermentation 2024324023

Texture: Fracture 26 25 32 force (g) Texture: Firmness 540 505 650 (g.mm) Viscosity at 50 s-1 416 415 400 (mPa.s) Appearance at Day Smooth, Soft Smooth, Soft Smooth, Soft 7 Appearance at Slight lumps and No lumps or specs Slight lumps and Month 3 specs are visible are visible specs are visible but but very minor very minor Example 10: 7% Protein Chilled Yoghurt

[00261] The following examples describe the production of yoghurt from a frozen milk concentrate according to the invention and compares the properties and sensory attributes of the yoghurts to that of yoghurts prepared from fresh milk combined with milk protein concentrates and whole milk powder by itself.

[00262] Samples were prepared similar to Example 8.

[00263] Analysis was done similar to the methods described in Example 8.

[00264] The results are shown in Table 11.

Table 11. Properties comparison between 7% Protein Chilled Yoghurt made from fresh milk, whole milk powder and frozen milk concentrates

Properties Yoghurt from fresh Yoghurt from whole Yoghurt from frozen milk combined with milk powder milk concentrates milk protein concentrates

pH post- 4.24 4.19 4.34 fermentation Texture: Fracture 205 155 203 force (g) Texture: Firmness 4490 3075 4200 (g.mm) 2024324023

Viscosity at 50 s-1 5270 2505 3800 (mPa.s) Appearance at Day Thick, Rough Thick, Smooth Thick, Smooth 7 texture Appearance at Day Thick, Rough Thick, Smooth Thick, Smooth 42 texture Example 11: UHT whole milk

[00265] The following example describes the production of a single strength UHT milk from a frozen milk concentrate and compares it with UHT milks prepared either from fresh milk or reconstituted whole milk powder.

[00266] Preparation method is as follows:

1. Weigh out 200 g of frozen milk concentrate or 126 g of whole milk powder per liter of final volume to give a milk containing 12-13% total solids (approximately 3.2% protein and 3.4% fat). 2. Add water to the mixer at 55°C, 790 g of water per 200 g FWMC or 880 g water per 126 g WMP. 3. Break the frozen blocks into 200-300 g pieces using a block cutter, add the frozen pieces or milk powder to the mixer. Set the mixer blade to 20 Hz. 4. Mix with recirculation for 30 minutes. 5. Pass approximately 5L through a sieve to check for undissolved lumps. If any lumps are found, recirculate for a further 10 minutes. 6. Check the total solids and adjust to 12-13% with water at 55°C. 7. Homogenize at 55-60°C, 200 bar 1st stage, 50 bar 2nd stage (250 bar total). 8. UHT treat at 142°C, 4 seconds, homogenize post UHT 150 bar 1st stage 50 bar 2nd stage (200 bar total). 9. Cool to 20-25°C and pack aseptically.

[00267] Samples were analyzed for foreign matter and for sterility at 30 and 55°C. They were also analyzed for Total solids, Ash by thermographic analysis, fat by the

Roese-Gottleib method, protein by Kjeldahl (total nitrogen x 6.38) and pH. Carbohydrate was calculated by difference.

[00268] Steam frothing of the UHT milks was assessed on 250 g samples of chilled (4-6°C) milk using a Nespresso Creatista plus machine equipped with steam wand. Samples were frothed using steam protocol 8, Hot setting, and assessed for boundary time (the time to form a distinct boundary between milk and froth) foam volume at 2 2024324023

minutes and relative foam stability (the amount of foam remaining after 2 minutes as a percentage of the foam volume at 2 minutes).

[00269] Samples were dispensed into clear PET bottles with 0.02% sodium azide added to prevent microbial growth and stored at 25°C. At 3 and 5 months, the milk was carefully decanted off and any sediment remaining was weighed and calculated as a percentage of the total milk.

[00270] All milks were sterile and free from foreign matter. Compositions were as shown below.

Table 12. Compositions of UHT milks made with reconstituted WMP and FWMC

Sample UHT milk from WMP UHT milk from UHT milk from fresh FWMC milk Total solids 12.84 12.55 11.47 Ash 0.64 0.60 0.67 Fat 3.47 3.49 3.26 Protein (TN x 6.38) 3.14 3.34 3.04 Carbohydrate 5.6 5.1 4.5 (by difference) pH 6.64 6.71 6.63

[00271] Steam frothing performance of milks are shown in Table 13.

Table 13. Steam frothing properties of UHT milks made with WMP and FWMC

Sample UHT milk from WMP UHT milk from UHT milk from fresh FWMC milk Boundary time (s) 88 123 129

Foam volume at 2 145 175 155 min (mL) Foam volume 72 83 77 stability (%)

[00272] Sediments in UHT milks after storage at 25°C are shown in Table 14.

Table 14. Sediment in UHT Milks made with WMP and FWMC 2024324023

Sample UHT milk from WMP UHT milk from UHT milk from fresh (%) FWMC (%) milk (%) 3 months 0.17 0 0 5 months 0.26 0 0 Example 12: Pasteurized double strength milk for barista applications

[00273] The following describes the production of a double strength pasteurized milk for barista applications from frozen milk concentrate according to the invention.

[00274] Preparation method

1. Weigh out 300 g of FWMC, 37 g of skim milk powder and 663 g of water per liter of product to give a milk containing 21-22% total solids with 6.2-6.3% protein and 5.0-5.2% fat. 2. Add water to the mixer and heat to 55°C. 3. Break the frozen blocks into small pieces using a block cutter, add the frozen pieces and skim milk powder to the mixer. Alternatively, thaw frozen block for 1 hour in a 60°C water bath and transfer partially thawed material to mixer. 4. Stir at low speed until the lumps have melted, then at higher speed for a further 30 minutes. 5. Pass through a sieve to check for undissolved lumps. If any lumps are found, stir for a further 10 minutes. 6. Heat to 70°C and homogenize at 200 bar 1st stage, 50 bar 2nd stage (250 bar total). 7. Heat at 95°C for a further 1 minute. 8. Cool rapidly to 20-25°C and pack into PET bottles and transfer to refrigerator. 9. Use within 1 week.

[00275] This assessment requires a standard espresso machine and 15-18 g of espresso ground coffee beans per shot.

[00276] Milks (160 mL) were poured into chilled 200-mL glasses and allowed to equilibrate in the refrigerator. Coffee (20-25 mL) was dispensed directly from the espresso machine onto the top of the milk and assessed for formation of clean layers.

Example 13: Recombined evaporated milk from WMP or frozen whole milk concentrate. 2024324023

[00277] The following describes the production of a recombined evaporated milk from frozen milk concentrate according to the invention.

[00278] Preparation method is as follows:

1. Weigh out 470 g of frozen whole milk concentrate to 540 g of water or 290 g of whole milk powder to 710 g of water per liter of recombined evaporated milk (28% total solids). 2. Add water to the mixer at 55°C 3. Break the frozen blocks into small pieces using a block cutter, add the frozen pieces or milk powder to the mixer. Alternatively, thaw frozen block for 1 hour in a 60°C water bath and transfer partially thawed material to mixer. 4. Stir at low speed until the temperature reaches 60°C and all lumps have melted, then add 0.2% lecithin at higher speed for a further 60 minutes. 5. Heat to 95°C and maintain for 10 minutes. 6. Cool to 55-60°C and homogenize at 160 bar 1st stage, 40 bar 2nd stage (200 bar total). 7. Cool rapidly to 20-25°C. 8. Pack into cans or Schott bottles. 9. Add 10% solutions of either anhydrous monosodium or anhydrous disodium phosphate in water as follows: 3M = 3mL MSP/400 mL, 2M = 2mL MSP/400 mL, 1M = 1mL MSP/400 mL, 0 = neither MSP nor DSP, 1D = 1 mL DSP/400 mL, 2D = 2mL DSP/400 mL, 3D = 3mL DSP/400 mL 10. Retort at 115°C for 15 minutes. Cool and check for aggregation by the spoon test 11. Smooth textured samples free of lumps or grains may be tested using the coffee aggregation test below.

[00279] The coffee sediment test was performed as follows: 1.7 g of instant coffee was dissolved in boiling water, and 45 mL of coffee solution was added to each of two 50 mL graduated centrifuge tubes. REM (5 mL) was added immediately to each tube and the tubes were mixed by inversion, centrifuged at 164g for 5 minutes and the volume of sediment assessed.

[00280] All samples of retorted REM were smooth textured and free from lumps or grains. All samples had minimal sediment as assessed by the coffee test.

Example 14: Recombined sweetened condensed milk from WMP or frozen whole milk concentrate.

[00281] The following describes the production of a recombined sweetened 2024324023

condensed milk from frozen milk concentrate according to the invention.

[00282] Preparation method is as follows:

1. Weigh out 530 g of FWMC to 30 g of water, or 320 g of WMP to 250 g of water per kilogram of final product. 2. Add water to the mixer and heat to 55°C. 3. Break the frozen blocks into small pieces using a block cutter, add the frozen pieces or milk powder to the mixer. Alternatively, thaw frozen block for 1 hour in a 60°C water bath and transfer partially thawed material to mixer. This will give a final product containing approximately 8% protein, 9% fat and 23-24% Milk solids-non- fat. 4. Stir at low speed until the temperature reaches 60°C and the concentrate is completely melted and smooth, then at higher speed for a further 60 minutes. 5. Add 430 g of granular sucrose per kilogram of final product (this will give a sugar number between 62 and 64 according to the formula 100*sucrose/ (sucrose + water)). 6. Continue to stir for a further 60 minutes. 7. Heat to 60°C and homogenize at 60 bar (second stage only). 8. Heat to 90°C and hold for 30 seconds. 9. Cool with stirring to 30-32°C, add 0.05% seed lactose (finely ground lactose). 10. Continue to cool with stirring to 20-25°C. 11. Pack into sterile cans or PET bottles with minimal headspace.

[00283] Samples were assessed using the coffee sediment test as described in example 6.

[00284] All samples had <0.25 mL sediment/ as assessed by the coffee test (recommended limit 0.5 mL sediment per tube).

[00285] It is not the intention to limit the scope of the invention to the abovementioned examples only. As would be appreciated by a skilled person in the art,

many variations are possible without departing from the scope of the invention as set out in the appended claims.

Claims

WHAT WE CLAIM IS

1. A frozen milk concentrate comprising from about 14% to about 35% by weight total protein and at least about 20% by weight total milk solids, wherein the total protein comprises β-lactoglobulin of which less than about 40% by weight is denatured, and wherein from about 45 to about 90% of total milk solids-not-fat in the frozen milk 2024324023

concentrate is protein.

2. A frozen milk concentrate comprising at least about 51% by weight total milk solids and at least about 12% by weight total protein, wherein total protein in the frozen milk concentrate comprises β-lactoglobulin of which less than about 40% by weight is denatured.

3. The frozen milk concentrate of claim 2, comprising from about 51% to about 78% by weight total milk solids.

4. The frozen milk concentrate of any one of claims 1 to 3, wherein, following 24 hours storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a sample comprising 12% by weight total solids, and the sample is mixed at 55°C for 30 minutes at 400 rpm with an overhead stirrer to produce a solubilised liquid milk, the solubilised liquid milk comprises protein particles, wherein the D[3,2] of the protein particles is less than about 2 μm.

5. The frozen milk concentrate of any one of claims 1 to 4, wherein, following 24 hours storage at a temperature of -18°C or less, when the frozen milk concentrate is combined with water to provide a 12% total solids sample; 100 g of sample is mixed for 5 minutes at 50°C with an antifoaming agent in an automatic solubility index mixer; and 50 mL of sample is centrifuged twice for 5 min at 160 g at room temperature to produce a sedimented sample, the sedimented sample comprises less than about 0.5 mL/50 mL of visible sediment.

6. The frozen milk concentrate of any one of claims 1 to 5, wherein the total protein comprises at least about 10% by weight whey protein.

7. The frozen milk concentrate of any one of claims 1 to 6, comprising lipid and protein in a weight ratio of from 0.01:1 to 2:1.

8. A process for preparing a frozen milk concentrate, the process comprising

b) providing an evaporation system that comprises a falling film evaporator and 2024324023

optionally a thin film evaporator,

9. The process of claim 8, wherein step a) comprises heating the liquid milk at a temperature of less than about 85°C for less than about 50 seconds.

10. The process of claim 8 or claim 9, wherein the evaporation system comprises between two and five falling film effects.

11. The process of claim 10, wherein the evaporation system comprises

12. The process of any one of claims 8 to 11, wherein the evaporation system comprises falling film evaporation followed by thin film evaporation. 2024324023

13. The process of claim 12, wherein the evaporation system comprises a thin film evaporator having a boiling temperature of from about 45°C to about 70°C.

14. The process of any one of claims 8 to 13, wherein the process comprises cooling the concentrated milk at a shear rate in step d) of at least 10 s-1.

15. The process of any one of claims 8 to 14, wherein the process comprises cooling the concentrated milk in a scraped surface heat exchanger.

16. The process of any one of claims 8 to 15, wherein cooling comprises introducing the concentrated milk into a scraped surface heat exchanger comprising a first barrel with a temperature of about -8°C to 10°C and a second barrel with a temperature of about -10°C to 5.5°C.

17. A process for preparing a frozen milk concentrate, the process comprising

a) providing a milk protein concentrate (MPC) comprising at least about 15% by weight total solids and at least about 12% by weight total protein,

f) freezing the cooled milk concentrate to a temperature of less than about - 10°C, preferably less than about -18°C, to provide a frozen milk concentrate; 2024324023

18. A frozen milk concentrate obtained by the process of any one of claims 8 to 17.

WO wo 2025/037250 PCT/IB2024/057867 1/1 1/1

FIGURE 1

Liquid milk MPC

Preheating

Pre heated milk or MPC

Evaporation

Concentrate

Cooling

Chilled

concentrate concentrate

Freezing

Frozen concentrate concentrate

Storage < -18°C