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Title:
A FORMULATION
Document Type and Number:
WIPO Patent Application WO/2017/072502
Kind Code:
A1
Abstract:
The present invention relates to formulations comprising a liquid such as an oil loaded onto a solid carrier, and methods for producing the same. The formulations can be used in foodstuffs, feeds, and cosmetic and industrial products. More specifically, the present invention relates to a formulation comprising a liquid loaded onto a particulate product comprised of particles which contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative,and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites.

Inventors:
VAN DEN ABBEELE RONY (BE)
MASSET JACQUES (GB)
Application Number:
PCT/GB2016/053327
Publication Date:
May 04, 2017
Filing Date:
October 26, 2016
Export Citation:
Click for automatic bibliography generation   Help
Assignee:
TATE & LYLE TECH LTD (GB)
International Classes:
A23L33/115; A23D9/00; A23K40/30; A23L27/00; A23P10/30; A23P10/40; A23P20/10; A61K8/11; A61K9/16; A61K9/50; A61K9/51
Domestic Patent References:
WO2009133409A12009-11-05
WO2013124652A12013-08-29
WO2015015151A12015-02-05
Foreign References:
US6159504A2000-12-12
US20130280409A12013-10-24
US20140113826A12014-04-24
EP0470872A11992-02-12
AU2013101255A42013-12-19
Attorney, Agent or Firm:
NIEUWENHUYS, William (GB)
Download PDF:
Claims:
CLAIMS:

1. A formulation comprising a liquid loaded onto a particulate product comprised of particles which contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative, and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites.

2. The formulation according to Claim 1 , wherein the particulate product has an average particle size by volume of about 600 μηι. 3. The formulation according to Claim 2, wherein the size of the particles ranges from about 5 μηι to about 1 100 μηι.

4. The formulation according to Claim 2 or Claim 3, wherein at least about 90% by volume of the particles of the particulate product have a size less than about 1 100 μηι.

5. The formulation according to Claim 1 , wherein particles of the particulate product are equal to or less than about 500 μηι in size.

6. The formulation according to Claim 1 or Claim 5, wherein at least about 95% by volume of the particles of the particulate product have a size less than about 500 μηι.

7. The formulation according to any one of Claims 1 , 5 and 6, wherein the particulate product has an average particle size by volume of about 200 μηι. 8. The formulation according to any one of Claims 1 and 5 to 7, wherein at least about 90% by volume of the particles of the particulate product have a size less than about 500 μηι.

9. The formulation according to any one of Claims 1 and 5 to 8, wherein at least about 95% by volume of the particles of the particulate product have a size less than about 200 μι ι. 10. The formulation according to any one of Claims 1 and 5 to 9, wherein at least about 95% by volume of the particles of the particulate product have a size less than about 100 μηι.

11. The formulation according to any one of Claims 1 , 5, 6 and 8 to 10, wherein at least about 95% by volume of the particles of the particulate product have a size less than about 50 μηι.

12. The formulation according to any one of Claims 1 , 5, 6 and 8 to 11 , wherein the particles of the particulate product have an average particle size by volume in the range of about 5 μηι to about 30 μηι.

13. The formulation according to Claim 12, wherein the particles of the particulate product have an average particle size by volume in the range of about 15 μηι to about 25 μι ι.

14. The formulation according to Claim 13, wherein the particulate product has an average particle size by volume of 20 μηι.

15. The formulation according to Claim 12, wherein the particles of the particulate product have an average particle size by volume in the range of about 20 μηι to about

30 μι ι.

16. The formulation according to Claim 15, wherein the particulate product has an average particle size by volume of 25 μηι.

17. The formulation according to any one of Claims 12 to 16, wherein at least about 90% by volume of the particles of the formulation have a size less than about 70 μηι.

18. The formulation according to Claim 17, wherein substantially all particles of the particulate product have a size by volume that is less than about 60 μηι.

19. The formulation according to any one of Claims 1 to 18, wherein the particles of the particulate product comprise a minor proportion by weight of the organic material. 20. The formulation according to Claim 19, wherein the particles of the particulate product comprise up to about 20% by weight of the organic material.

21. The formulation according to any one of Claims 1 to 20, wherein the liquid is present in an amount of equal to or less than 120% by weight relative to the weight of the particulate product.

22. The formulation according to any one of Claims 1 to 21 , wherein the liquid is present in an amount of equal to or less than 100% by weight relative to the weight of the particulate product.

23. The formulation according to any one of Claims 1 to 22, wherein the liquid is present in an amount of equal to or less than 80% by weight relative to the weight of the particulate product. 24. The formulation according to any one of Claims 1 to 23, wherein the liquid is present in an amount of equal to or less than 60% by weight relative to the weight of the particulate product.

25. The formulation according to any preceding claim, wherein the liquid is selected from the group consisting of an oil, a water-oil emulsion, a water-based liquid, propylene glycol, polypropylene glycol, glycerine or 1 , 3-propane diol.

26. The formulation according to Claim 25, wherein the liquid is an oil. 27. The formulation according to Claim 26, wherein the oil is one or more selected from the group consisting of essential oils, oleoresins, oil-based colourings, vegetable oils, animal fats or oils, vitamin oils and oily additives.

28. The formulation according to any preceding claim, wherein the particulate product is a particulate salt product comprised of particles which contain one or more of sodium chloride and potassium chloride, and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride and potassium chloride attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites.

29. The formulation according to Claim 28, wherein the particulate product is a particulate salt product comprised of particles which contain sodium chloride and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of sodium chloride attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites.

30. The formulation according to any one of Claims 1 to 29, wherein the formulation is in the form of a powder.

31. The formulation according to Claim 30, wherein the powder is a free-flowing powder. 32. The formulation according to any one of Claims 1 to 31 , wherein the average particle size by volume of the formulation is in the range of about 10 μηι to about 600 μηι.

33. A method of preparing a formulation comprising the step of blending a liquid with a particulate product, wherein the particulate product is comprised of particles which contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative, and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites.

34. The method according to Claim 33, wherein the method is for preparing a formulation according to any one of Claims 1 to 32.

35. The method according to Claim 33 or 34, wherein the particulate product is as defined according to any one of Claims 2 to 18, 28 and 29. 36. The method according to any one of Claims 33 to 35, wherein the liquid is selected from the group consisting of an oil, a water-oil emulsion, a water-based liquid, propylene glycol, polypropylene glycol, glycerine or 1 , 3-propane diol.

37. The method according to Claim 36, wherein the liquid is an oil.

38. The method according to Claim 37, wherein the oil is one or more selected from the group consisting of essential oils, oleoresins, oil-based colourings, vegetable oils, animal fats or oils, vitamin oils and oily additives. 39. The method according to any one of Claims 33 to 38, wherein the liquid is mixed with the particulate product prior to the blending step.

40. The method according to any one of Claims 33 to 39, wherein the liquid is gradually dosed onto the particulate product during the blending step.

41. The method according to Claim 40, wherein the liquid is sprayed onto the particulate product during the blending step.

42. The method according to any one of Claims 33 to 41 , wherein a solvent is added to the liquid prior to blending or mixing with the particulate product.

43. The method according to Claim 42, wherein the solvent is one or more selected from the group consisting of a medium chain triglyceride and an alcohol. 44. The method according to any one of Claims 33 to 43, wherein the step of blending the liquid with the particulate product is performed in a vacuum.

45. The method according to any one of Claims 33 to 43, wherein the step of blending the liquid with the particulate product is performed in the presence of an inert atmosphere.

46. The method according to any one of Claims 33 to 45, wherein the step of blending the liquid with the particulate product is performed at ambient (room) temperature.

47. The method according to any one of Claims 33 to 45, wherein the step of blending the liquid with the particulate product is performed in the range from about 5 °C to about 15 °C. 48. A formulation prepared by the method according to any one of Claims 33 to 47.

49. A foodstuff comprising a formulation according to any one of Claims 1 to 32 and 48. 50. A feed comprising a formulation according to any one of Claims 1 to 32 and 48.

51. A cosmetic product comprising a formulation according to any one of Claims 1 to 32 and 48. 52. Use of a formulation according to any one of Claims 1 to 32 and 48 in a foodstuff, feed, cosmetic or industrial product.

53. Use of a particulate product in the production of a formulation according to any one of Claims 1 to 32 and 48, wherein the particulate product is comprised of particles which contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative, and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites.

Description:
A Formulation

Field of the Invention

The present invention relates to formulations comprising a liquid such as an oil loaded onto a solid carrier, and methods for producing the same. The formulations can be used in foodstuffs, feeds, and cosmetic and industrial products.

Background of the Invention It is commonly accepted that liquid ingredients, such as oils, are difficult to handle. On a large scale, more care and thought is required when storing and transporting liquids in comparison to solid products. On a smaller scale, when a low dosage of a concentrated liquid is required in a final application, accurate dosing can prove difficult, particularly when dealing with viscous liquids. In addition, significant wastage can occur in the handling and transport of viscous liquids, especially in the period between manufacture and use in a final application. Furthermore, in the case of oils and oily liquids, problems can arise when they are used in water-based applications as there is a tendency for the oil and water phases to separate. Accordingly, formulations in which liquids, especially oils, are loaded onto a carrier are generally preferred by industry in order to reduce wastage and increase the ease of handling, thus reducing costs and increasing efficiency.

There are a number of currently available methods to convert oils into a powder form. However, all of these methods suffer from limitations that restrict their utility. For example, it is known that oils can be plated on conventional carriers such as regular salt, maltodextrin, lactose and native starch. By way of background, the term "plated" refers to the common process which consists in depositing a liquid on a solid carrier material to obtain a powder form of said liquid. Plating oils on conventional carriers can only achieve limited loading of between about 5 and 10% by weight (even in the presence of an anti-caking agent) before clumping of the carrier occurs to give a sticky, non-free-flowing powder. In addition, lactose, which is a dairy allergen and presents some intolerance, and genetically modified starches do not meet some specific market requirements. Another method involves spray drying oils with a carrier such as acacia gum, maltodextrin and modified starch. This method can achieve slightly higher oil loadings of 20 to 25% by weight. However, the high temperatures required in this process can damage sensitive oils, cause loss of volatiles, lead to flavour profile changes and loss of functionality, meaning that the spray drying processes cannot be universally applied to all oils. Furthermore, spray drying processes are expensive due to the energy and equipment required. Also, in respect of downstream processing, incorporating a spray dried powder product into a blend of other ingredients requires at least one additional processing step in a different piece of equipment.

Oils can also be plated on non-conventional carriers such as silicon dioxide or porous starch.

Porous starches (e.g. Starrier™ that is marketed by Cargill) can achieve good oil loadings (e.g. up to about 60 g of oil per 100 g of starch). However, plating viscous oils on porous starch is problematic as clumping occurs and should therefore be avoided. Another disadvantage of using porous starch is that it is not fully soluble. This can have the undesired result that the release of the oil into the end application is delayed or incomplete. Its poor solubility can also mean that the texture and visual aspect of an end product are impacted. Powder forms of oils plated on porous starch may also have to be labelled as starch and its use limited in certain applications depending on regulatory concerns. Finally, the use of starch could bring with it an undesired aftertaste. Silicon dioxide can achieve high oil loadings, but the use of silicon dioxide as a carrier is often limited by regulations and does not present a clean label solution. There is also uncertainty as to whether silicon dioxide will be classified as nanotechnology in future.

It is an object of the present invention to obviate or mitigate the above mentioned problems and disadvantages. Summary of the Invention

According to an aspect of the present invention, there is provided a formulation comprising a liquid loaded onto a particulate product. Preferably, the formulation is in the form of a powder.

The particulate product that can be used in the present invention comprises particles that contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative), and an organic material that is a solid at ambient temperature (e.g. 15 °C to 35 °C or 15 °C to 25 °C). The particles have a structure that is comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative attached together within the particles. In addition, at least a proportion of the particles are hollow and are formed of an outer shell of the crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative).

In an embodiment, the particulate product has an average particle size by volume of 600 μηι, with a broad particle size range (e.g. from about 5 μηι to about 1 100 μηι). Preferably, at least about 90% by volume of the particles of the particulate product have a size less than about 1 100 μηι.

In an embodiment, particles of the particulate product are equal to or less than about 500 μηι in size. Preferably, at least about 95% by volume of the particles of the particulate product have a size less than about 500 μηι. In another embodiment, at least about 95% by volume of the particles of the particulate product have a size less than about 200 μηι.

In another embodiment, the particulate product has an average particle size by volume of about 200 μηι. Preferably, at least about 90% by volume of the particles of the particulate product have a size less than about 500 μηι. For example, the particulate product may be provided by the product commercially available under the name SODA-LO® Fine N, which has an average particle size by volume of about 200 μηι.

In a further embodiment, at least about 95% by volume of the particles of the particulate product have a size less than about 100 μηι.

In yet another embodiment, at least about 95% by volume of the particles of the particulate product have a size less than about 50 μηι. In other embodiments, the particles of the particulate product have an average particle size by volume in the range of about 5 μηι to about 30 μηι, e.g. in the range of about 15 μηι to about 25 μηι or about 20 μηι to about 30 μηι, and preferably are of narrow particle size distribution. In an embodiment, at least about 90% by volume of the particles of the particulate product have a size less than about 70 μηι. Preferably, substantially all particles of the particulate product have a size by volume that is less than 60 μηι. For example, the particulate product may be provided by the product commercially available under the name SODA-LO® Extra Fine (or SODA-LO® Extra Fine M) which is produced in accordance with the teachings of WO 2009/133409 and which has an average particle size by volume of about 20 μηι to about 30 μηι.

The particles of the particulate product preferably comprise a minor proportion by weight of the organic material. More preferably, the particles of the particulate product comprise up to about 20% by weight of the organic material. In an embodiment, the liquid is present in an amount of equal to or less than 60% by weight relative to the weight of the particulate product. In other words, for every 100 g of the particulate product, 60 g of liquid is loaded onto said particulate product.

In another embodiment, the liquid is present in an amount of equal to or less than 80% by weight relative to the weight of the particulate product.

In yet another embodiment, the liquid is present in an amount of equal to or less than 100% by weight relative to the weight of the particulate product. In a further embodiment, the liquid is present in an amount of equal to or less than 120% by weight relative to the weight of the particulate product.

In an embodiment, the liquid is selected from the group consisting of an oil, a water-oil emulsion, a water-based liquid, propylene glycol, polypropylene glycol, glycerine or 1 , 3-propane diol. Preferably, the liquid is an oil. The oil is preferably one or more selected from the group consisting of essential oils, oleoresins, oil-based colourings, vegetable oils, animal fats or oils, vitamin oils and oily additives. In preferred embodiments, the average particle size by volume of the formulation is in the range of about 10 μηι to about 600 μηι (e.g. about 10 μηι to about 500 μηι).

Preferably, the particulate product is a particulate salt product comprised of particles which contain one or more of sodium chloride and potassium chloride, and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride and potassium chloride attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites. More preferably, the particulate product is a particulate salt product comprised of particles which contain sodium chloride and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of sodium chloride attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites.

According to another aspect of the present invention, there is provided a method of preparing a formulation, wherein the method comprises the step of blending a liquid with a particulate product, and wherein the particulate product comprises particles that contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative), and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative) attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites. The above summary relating to the particulate product applies mutatis mutandis to the method.

In an embodiment, the liquid is mixed with the particulate product prior to the blending step. In an embodiment, the liquid is gradually dosed onto the particulate product during the blending step. For example, the liquid is sprayed onto the particulate product during the blending step.

In an embodiment, a solvent is added to the liquid prior to the step of blending or mixing the liquid with the particulate product. Preferably, the solvent is selected from a medium chain triglyceride or an alcohol.

In an embodiment, the step of blending the liquid with the particulate product is performed in a vacuum. In another embodiment, the step of blending the liquid with the particulate product is performed in the presence of an inert atmosphere.

In an embodiment, the step of blending the liquid with the particulate product is performed at ambient (room) temperature. In another embodiment, the step of blending the liquid with the particulate product is performed in the range from about 5 °C to about 15 °C.

According to another aspect of the present invention, there is provided the use of a particulate product in the production of a formulation in accordance with the present invention, wherein the particulate product is comprised of particles which contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative), and an organic material that is a solid at ambient temperature, and which have a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative) attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites. The above summary relating to the particulate product applies mutatis mutandis to this aspect of the invention.

According to another aspect of the present invention, there is provided the use of the formulation in food, feed, cosmetic or industrial products. According to a further aspect of the invention, there is provided a foodstuff, a feed, a cosmetic product or an industrial product comprising the formulation of the present invention.

Brief Description of the Drawings

Figure 1 shows the outcome of loading the salt samples with sunflower oil in Example 1.

Figure 2 shows the outcome of loading the salt samples with a combination of sunflower oil and paprika oleoresin in Example 2.

Figure 3A shows the outcome of the centrifugation test of Example 3 when 3.0 g of sunflower oil was centrifuged with 2.5 g of regular kitchen salt. Figure 3B shows the outcome of the centrifugation test of Example 3 when 3.0 g of sunflower oil was centrifuged with 2.5 g of SODA-LO® Extra Fine M.

Figure 4A is an image of regular kitchen salt dosed with 15% by weight of liquid pepper flavour in accordance with Example 4.

Figure 4B is an image of SODA-LO® Extra Fine M dosed with 15% by weight of liquid pepper flavour in accordance with Example 4.

Figure 5 is a scanning electron microscopy (SEM) image of the particles produced in Preparation Example 1. Figure 6 shows scanning electron microscopy (SEM) images of the particles produced in Preparation Example 2.

Figure 7 is a scanning electron microscopy (SEM) image of the particles produced in Preparation Example 3.

Figure 8 is a scanning electron microscopy (SEM) image of the particles produced in Preparation Example 4. Figure 9 is a scanning electron microscopy (SEM) image of the particles produced in Preparation Example 5.

Figure 10 is a scanning electron microscopy (SEM) image of the particles produced in Preparation Example 6.

Figures 1 1A to 1 1 1 are scanning electron microscopy (SEM) images of the particles produced in Preparation Example 7.

Detailed Description

The present invention relates to the finding that a particular form of particulate product can efficiently convert liquids (e.g. oils) into powder form, in particular, a free-flowing powder. Advantageously, formulations can be obtained with loading capacities that exceed currently available powder formulations of liquids (e.g. oils). In the formulations of the present invention, the liquid is loaded onto the particulate product. In other words, the particulate product acts as a carrier for the liquid.

Particulate products that can be used in the present invention contain particles that comprise: one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative; and an organic material that is a solid at ambient temperature (e.g. from about 15 °C to about 35 °C or from about 15 °C to about 25 °C). For example, the particulate products may contain particles that comprise: one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative; and an organic material that is a solid at ambient temperature. The particles of the particulate product may comprise a minor proportion by weight (e.g. up to about 20% by weight) of the organic material and have a structure comprised of individual crystallites of one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative), attached together within the particles.

Additionally, the particulate product comprises at least a proportion of hollow particles comprised of an outer shell formed of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative) attached together to form the shell, which itself surrounds the hollow interior cavity of the particle.

These hollow particles may be termed "microspheres". The shell may be "complete" in the sense that the hollow interior cavity is fully encased by the shell. Alternatively, the shell may not be fully complete. The structure of the hollow particles and the individual crystallites may readily be visualised under a Scanning Electron Microscope at an appropriate magnification (e.g. x5000).

Examples of phosphates that can be used in the present invention include, but are not limited to, calcium phosphate and sodium phosphate. Examples of carbonates that can be used in the present invention include, but are not limited to, sodium bicarbonate and potassium bicarbonate. In certain embodiments, the carbonate is not calcium carbonate.

A non-limiting example of a sulfate that can be used in the present invention is calcium sulfate.

Examples of cellulose derivatives that can be used in the present invention include, but are not limited to, microcrystalline cellulose. The particles contained in the particulate product may comprise a blend of two or more salts selected from sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative. For example, the particles may comprise a blend of two salts selected from sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative. In embodiments in which the particles comprise a blend of two or more salts, the two or more salt components may be present in equal or unequal amounts by weight with respect to each other. The particles may comprise a blend of two or more salts selected from the group consisting of sodium chloride, potassium chloride, calcium chloride and sodium bicarbonate. For example, the particles may comprise a blend of: sodium chloride and potassium chloride; sodium chloride and calcium chloride; sodium chloride and sodium bicarbonate; potassium chloride and calcium chloride; potassium chloride and sodium bicarbonate; or calcium chloride and sodium bicarbonate. Alternatively, the particles may comprise a blend of: sodium chloride, potassium chloride and calcium chloride; sodium chloride, potassium chloride and sodium bicarbonate; sodium chloride, calcium chloride and sodium bicarbonate; or potassium chloride, calcium chloride and sodium bicarbonate. Further, the particles may comprise a blend of: sodium chloride, potassium chloride, calcium chloride and sodium bicarbonate.

In an embodiment, the particles comprise a blend of sodium chloride with one or more of potassium chloride, calcium chloride and sodium bicarbonate. Preferably, the sodium chloride is present in an amount from 50% to 99% by weight relative to the total weight of the sodium chloride, potassium chloride, calcium chloride and sodium bicarbonate present in the particles. For example, the sodium chloride may be present in an amount from 50% to 90%, from 50% to 80%, from 60% to 80% or from 70% to 80% by weight relative to the total weight of the sodium chloride, potassium chloride, calcium chloride and sodium bicarbonate present in the particles.

For example, when the particles comprise a blend of sodium chloride and one of potassium chloride, calcium chloride and sodium bicarbonate, the sodium chloride may be present in an amount from 50% to 99% by weight, and the one of potassium chloride, calcium chloride and sodium bicarbonate may be present in an amount from 1 % to 50% by weight relative to the total weight of the sodium chloride and one of potassium chloride, calcium chloride and sodium bicarbonate present in the particles. In certain embodiments, the particles comprise a blend of sodium chloride and potassium chloride. The hollow particles of the particulate product preferably comprise at least 30% of the particles in the particulate product, more preferably at least 40% and still more preferably comprise a substantial proportion of the particulate product, i.e. more than 50%. The proportion of hollow particles is preferably at least 60%, more preferably at least 70% and even more preferably at least 80% and still more preferably at least 90% of the particulate product. The ideal is 100%, but in practice the particulate product may comprise 50-90% of the hollow particles. The percentage of hollow particles may be assessed on a numerical basis by examining the particulate product under a suitable magnification (e.g. using a scanning electron microscope) and counting the number of hollow particles as compared to the number of any solid particles. Generally a magnification of x500 to x2000 will be suitable for this purpose, although the skilled person can readily select the most appropriate value.

The organic material, which forms a component of the particles (hollow or otherwise) of the particulate product is preferably partially, and ideally substantially, soluble in water. The material may, for example, be Gum Arabic. The material may, for example, be malic acid. The material may, for example, be a natural or synthetic polymer. The material may, for example, be a carbohydrate, e.g. an oligosaccharide or a polysaccharide. Alternatively, the material may be a protein, for example, hydrolysed vegetable protein. The material may also be yeast extract (e.g. high nucleotide yeast extract).

Mixtures of such polymer types can also be used. If the polymer is a carbohydrate then it may, for example, be one or more of maltodextrin (e.g. Fibresol®), Gum Arabic, starch (e.g. soluble corn starch, potato starch or soya bean starch), hydroxypropyl cellulose, Merigel™ (starch), Mira-Mist® SE (Modified Starch), Promitor® L70 (Soluble gluco fibre), Locust Bean Gum (Genu gum), Maltosweet™ 120 (Maltodextrin), Gellan Gum, Low Acyl (Kelcogel® F), Pullulan, Xanthan Gum (Keltrol® T) and Pectin (Genu pectin). In certain preferred embodiments, the organic material is one or more of Gum Arabic and maltodextrin. In preferred embodiments, the organic material is one or more selected from Gum Arabic, guar gum, carrageenan, agar, polyethylene glycols (e.g. having a molecular weight in the range of 3,000-20,000), soluble gluco fibre (e.g. Promitor® L70), alginate, propylene glycol alginate (e.g. Protanal Ester), pullulan (e.g. PI-20), maltodextrin (e.g. Fibresol®, Star-Dri®1 , Star-Dri®10 or Maltosweet™ 120), starch (e.g. corn starch, soluble corn starch, potato starch, soya bean starch octanylsuccinate starch (Purity Gum® 2000), Mira-Cap® lipophilic starch, Mira-Mist® 662, Mira-Mist® SE or Merigel™), hydrolysed vegetable protein, hydroxypropyl cellulose, carboxymethyl cellulose (e.g. CMC-9MF), gellan gum (such as low acyl gellan gum (e.g. Kelcogel® F) or high acyl gellan gum (e.g. Kelcogel® LT100)), high methoxyl pectin (D slow set pectin HM), Xanthan Gum (e.g. Keltrol® T) and Locust Bean Gum (e.g. Genu gum).

Examples of synthetic polymers that may be used include polyethylene glycol (although this will not be suitable if the formulation is for use in food applications). The polyethylene glycol may, for example, have a molecular weight in the range of 3,000- 20,000.

In an embodiment, the particles of the particulate product have an average particle size by volume of about 600 μηι. In this embodiment, the particle size range may be broad. For example, the size of the particles may range from about 5 μηι to about 1 100 μηι. In this embodiment, it is preferred that at least about 90% by volume of the particles of the particulate product have a size less than about 1 100 μηι.

Alternatively, the particles of the particulate product may have an average particle size by volume of about 500 μηι. The particles of the particulate product may be equal to or less than about 500 μηι in size. The particulate product may have a particle size such that at least about 95% by volume of the particles of the product have a size less than about 500 μηι (e.g. less than about 400 μηι or less than about 300 μηι), preferably less than about 200 μηι and more preferably less than about 100 μηι (e.g. less than about 50 μι ι).

In an embodiment, the particles have an average particle size by volume of about 200 μηι. In this embodiment, it is preferred that at least about 90% by volume of the particles of the particulate product have a size less than about 500 μηι. The particles of the particulate product may have an average particle size by volume in the range of about 5 μηι to about 30 μηι, e.g. in the range about 15 μηι to about 25 μηι (e.g. about 20 μηι), or about 20 μηι to about 30 μηι (e.g. about 25 μηι), and may be of narrow particle size distribution. By narrow particle size distribution, it is meant that the span (which is equal to (D90-D10)/D50) is from about 0.5 to about 1 .5. In an embodiment, at least about 90% by volume of the particles of the particulate product have a size less than about 70 μηι. Preferably, substantially all particles have a size less than 60 μηι. The formulation of the present invention preferably has an average particle size by volume in the range of about 10 μηι to about 600 μηι (e.g. about 10 μηι to about 500 μηι). The formulation may have a particle size such that at least about 90% by volume of the particles of the powder have a size less than about 1 100 μηι. The formulation may have a particle size such that at least about 95% by volume of the particles of the powder have a size less than about 500 μηι (e.g. less than about 400 μηι or less than about 300 μηι), preferably less than about 200 μηι, and more preferably less than about 100 μηι (e.g. less than about 50 μηι).

The formulation may have an average particle size by volume of about 200 μηι. In this embodiment, it is preferred that at least about 90% by volume of the particles of the formulation have a size less than about 500 μηι.

The particles of the formulation may have an average particle size by volume in the range of about 5 μηι to about 30 μηι, e.g. in the range of about 15 μηι to about 25 μηι (e.g. about 20 μηι) or in the range of about 20 μηι to about 30 μηι (e.g. about 25 μηι) and may be of narrow particle size distribution. In an embodiment, at least about 90% by volume of the particles of the formulation have a size less than about 70 μηι. Preferably, substantially all particles of the formulation have a size less than 60 μηι. Unless stated otherwise, particle sizes and particle size distributions as referred to herein for the particulate product and the formulations of the present invention are determined using an LS13 320 Laser Diffraction Size Analyser (ex Beckman Coulter). The term "average particle size by volume" means the average of the sum of particle sizes as measured for the entire volume of the sample tested. The particulate product may be produced by the steps of:

(i) providing a mixture which comprises one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative), and the organic material dissolved in a solvent, preferably water for the case where the organic material is water soluble; and

(ii) atomising the mixture to produce atomised droplets and evaporating the solvent (preferably water) from the atomized droplet to produce particles containing (i) the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative), and (ii) the organic material, and having a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative) attached together in the particle, which particles of said hollow product comprise hollow particles formed of an outer shell of the crystallites.

An elevated temperature may be used for evaporation of the solvent. For example, the evaporation may take place at a temperature from 50 °C to 350 °C, from 100 °C to 300 °C, from 100 °C to 250 °C or from 100 °C to 210 °C. The evaporation of the solvent may be effected using a hot air cyclone effect. For the purposes of obtaining the salt products referred to herein, different temperature values may be appropriate for different organic materials. For example, evaporation of the solvent when using maltodextrin may be effected at a temperature of 190 °C to 300 °C, for example, 190 °C to 200 °C (e.g. about 195 °C). Evaporation of the solvent when using Gum Arabic may be effected at a temperature of 135 °C to 250 °C, for example, 135 °C to 145 °C (e.g. about 140 °C). The appropriate temperature value may be determined by simple experiment and is well within the capability of the person skilled in the art. The mixture that is subjected to atomisation may contain 5% to 60% by weight of salt (e.g. sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative) based on the weight of the solvent. For example, the mixture may contain 5% to 55%, 10% to 55%, 15% to 55%, 20% to 55% or 25% to 55% by weight of salt based on the weight of the solvent. Alternatively, the mixture may contain 5% to 50%, 5% to 40%, 10% to 40% or 20% to 40% by weight of salt based on the weight of the solvent. Alternatively or additionally, the mixture may contain 0.1 % to 20% by weight of the organic material based on the weight of the solvent. For example, the mixture may contain 0.1 % to 10% or 0.3% to 7% by weight of the organic material based on the weight of the solvent. The mixture may be a fully solubilised solution or a slurry.

Step (ii) may be effected by spray drying. The spray drying may be effected using a conventional spray drying apparatus. For example, for the purposes of small batches of the salt product, a Buchi Mini Spray Dryer B-290 is suitable. Niro industrial dryers, or other commercial spray dryers, may be used for commercial production of the salt product. In a preferred embodiment of the present invention, the particulate product is a particulate salt product, wherein the salt is preferably sodium chloride (NaCI) or potassium chloride (KCI). In particularly preferred embodiments, the particulate salt product is a particulate sodium chloride product. Other salts that may be contemplated in the present invention include sodium bicarbonate.

Particulate salt products that can be used in the present invention contain particles that comprise salt (e.g. sodium chloride or potassium chloride) and an organic material that is a solid at ambient temperature (e.g. from about 15 °C to about 35 °C or from about 15 °C to about 25 °C). The particles of the salt product may comprise a minor proportion by weight (e.g. up to about 20% by weight) of the organic material and have a structure comprised of individual crystallites of salt (e.g. sodium chloride or potassium chloride) attached together within the particles. Additionally, as disclosed above in relation to the particulate products in general, the salt product comprises at least a proportion of hollow particles comprised of an outer shell formed of individual crystallites of salt attached together to form the shell, which itself surrounds the hollow interior cavity of the particle. These hollow particles may be termed "microspheres". The shell may be "complete" in the sense that the hollow interior cavity is fully encased by the shell. Alternatively, the shell may not be fully complete. The structure of the hollow particles and the individual crystallites may readily be visualised under a Scanning Electron Microscope at an appropriate magnification (e.g. x5000).

Due to its hollow sphere structure, the particulate salt product has a much lower bulk density compared to the regular salt (e.g. regular sodium chloride or regular potassium chloride). Its surface of contact is therefore much higher. It is hypothesised that this higher surface of contact results in a much higher liquid (e.g. oil) loading capacity.

The hollow particles preferably comprise at least 30% of the particles in the particulate salt product, more preferably at least 40% and still more preferably comprise a substantial proportion of the particulate salt product, i.e. more than 50%. The proportion of hollow particles is preferably at least 60%, more preferably at least 70% and even more preferably at least 80% and still more preferably at least 90% of the particulate salt product. The ideal is 100%, but in practice the particulate salt product may comprise 50-90% of the hollow particles. The percentage of hollow particles may be assessed on a numerical basis by examining the particulate salt product under a suitable magnification (e.g. using a scanning electron microscope) and counting the number of hollow particles as compared to the number of any solid particles. Generally a magnification of x500 to x2000 will be suitable for this purpose, although the skilled person can readily select the most appropriate value. In an embodiment, the particles of the particulate salt product have an average particle size by volume of 600 μηι. In this embodiment, the particle size range may be broad. For example, the size of the particles may range from about 5 μηι to about 1 100 μηι. In this embodiment, it is preferred that at least about 90% by volume of the particles of the particulate salt product have a size less than about 1 100 μηι.

The particles of the particulate salt product may have an average particle size by volume of 500 μηι. The particles of the particulate salt product may be equal to or less than about 500 μηι in size. The particulate salt product may have a particle size such that at least about 95% by volume of the particles of the salt product have a size less than about 500 μηι (e.g. less than about 400 μηι or less than about 300 μηι), preferably less than about 200 μηι and more preferably less than about 100 μηι (e.g. less than about 50 μηι).

In an embodiment, the particles of the particulate salt product have an average particle size by volume of about 200 μηι. In this embodiment, it is preferred that at least about 90% by volume of the particles of the particulate salt product have a size less than about 500 μηι.

The particles of the particulate salt product may have an average particle size by volume in the range of about 5 μηι to about 30 μηι, e.g. in the range about 15 μηι to about 25 μηι (e.g. about 20 μηι) or in the range of about 20 μηι to about 30 μηι (e.g. about 25 μηι) and may be of narrow particle size distribution. By narrow particle size distribution, it is meant that the span (which is equal to (D90-D10)/D50) is from about 0.5 to about 1.5. In an embodiment, at least about 90% by volume of the particles of the particulate salt product have a size less than about 70 μηι. Preferably, substantially all particles have a size less than 60 μηι.

The particulate salt product may consist of particles which contain salt and the organic material that is a solid at ambient temperature. Alternatively, the particulate salt product may comprise such particles in admixture with salt particles (e.g. sodium chloride particles or potassium chloride particles) (i.e. salt that is not contained in a particle with the organic material). For example, the particulate salt product may comprise: (i) particles containing salt and the organic material that have an average particle size by volume in the range of about 5 μηι to about 30 μηι, e.g. in the range about 15 μηι to about 25 μηι (e.g. about 20 μηι) or in the range of about 20 μηι to about 30 μηι (e.g. about 25 μηι); and (ii) salt particles (e.g. sodium chloride particles or potassium chloride particles) having a size by volume up to a maximum of about 1100 μηι (e.g. up to maximum of about 1000 μηι, up to maximum of about 900 μηι, up to maximum of about 800 μηι, up to maximum of about 700 μηι, up to maximum of about 600 μηι or up to maximum of about 500 μηι).

The particulate salt product may be a salt product of the type disclosed in WO 2009/133409 A1 (Eminate Ltd) which also discloses a method of producing the salt product. The particulate salt product may also be a salt product of the type disclosed in WO 2015/015151 A1 (Tate & Lyle) as being used in the milling process described therein. The particulate salt product may also be a salt product of the type disclosed in WO 2015/015151 A1 (Tate & Lyle) as the salt product composition of the milling process described therein. The full disclosures of WO 2009/133409 A1 and WO 2015/015151 A1 are incorporated herein by reference. In WO 2009/133409 A1 and WO 2015/015151 A1 , the salt is sodium chloride.

The particulate salt product may be produced by the steps of:

(i) providing a mixture which comprises salt (e.g. sodium chloride or potassium chloride) and the organic material dissolved in a solvent, preferably water for the case where the organic material is water soluble; and

(ii) atomising the mixture to produce atomised droplets and evaporating the solvent (preferably water) from the atomized droplet to produce particles containing (i) salt, and (ii) the organic material, and having a structure comprised of individual crystallites of salt (e.g. sodium chloride or potassium chloride) attached together in the particle, which particles of said hollow product comprise hollow particles formed of an outer shell of the crystallites.

Step (ii) may be effected by spray drying.

In a preferred embodiment of the invention, the particulate salt product is provided by the products commercially available under the name SODA-LO® Extra Fine or SODA- LO® Extra Fine M, which have an average particle size by volume of about 20 μηι to about 30 μηι, wherein at least about 90% by volume of the particles of the particulate salt product have a size less than about 70 μηι, and wherein the salt is sodium chloride. In SODA-LO® Extra Fine, the organic material is Acacia gum, and in SODA- LO® Extra Fine M, the organic material is maltodextrin. A method for preparing SODA- LO® Extra Fine and SODA-LO® Extra Fine M is described in WO 2009/133409 A1.

In another embodiment of the invention, the particulate salt product is provided by the product commercially available under the name SODA-LO® Fine N which has an average particle size by volume of about 200 μηι, wherein at least about 90% by volume of the particles of the particulate salt product have a size less than about 500 μηι, and wherein the salt is sodium chloride. SODA-LO® Fine N may be prepared by a traditional two-step milling process in which salt crystals with an average particle size by volume greater than about 500 μηι are milled to give a powder with an average particle size by volume in the range 150 μηι to 250 μηι and the resulting powder is then mixed with SODA-LO® Extra Fine particles. Alternatively, SODA-LO® Fine N may be prepared by the method disclosed in WO 2015/015151 A1 which involves comminuting a first particulate fraction comprised of sodium chloride crystals having an average particle size by volume of at least 500 μηι, in the presence of a second particulate fraction which is a particulate salt product comprised of particles which contain (a) sodium chloride and (b) an organic material that is a solid at ambient temperature and which have a structure comprised of individual crystallites of sodium chloride attached together in the particles of the product wherein at least 95% by volume of the particles of the salt product have a size less than 100 μηι and wherein particles of the product comprise hollow particles formed of an outer shell of said crystallites.

In a further embodiment of the invention, the particulate sodium chloride product has an average particle size by volume of about 600 μηι. This particulate sodium chloride product may be prepared by a process in which sodium chloride crystals with an average particle size by volume greater than about 600 μηι is then mixed with SODA- LO® Extra Fine particles.

It is preferable to use SODA-LO® Extra Fine, SODA-LO® Extra Fine M, SODA-LO® Fine and SODA-LO® Fine N as carriers for a number of reasons. For example, these products are fully soluble, thus providing easy and full release of the liquid (e.g. oil) into the final application and/or during consumption. The good solubility also means that there is no impact on the texture of the final application, which is particularly advantageous in food applications.

In an embodiment, the liquid is present in an amount of equal to or less than 120% by weight relative to the weight of the particulate product in the formulation. In other words, for every 100 g of the particulate product, 120 g of liquid is loaded onto said particulate product. For example, the liquid may be present in an amount from 1 % to 120%, from 10% to 120%, from 20% to 120%, from 30% to 120%, from 40% to 120%, from 50% to 120%, from 60% to 120%, from 70% to 120%, from 80% to 120%, from 90% to 120%, from 100% to 120%, or from 1 10% to 120% by weight relative to the weight of the particulate product). In another embodiment, the liquid is present in an amount of equal to or less than 100% by weight relative to the weight of the particulate product (e.g. from 1 % to 100%, from 10% to 100%, from 20% to 100%, from 30% to 100%, from 40% to 100%, from 50% to 100%, from 60% to 100%, from 70% to 100%, from 80% to 100%, or from 90% to 100% by weight). In yet another embodiment, the liquid is present in an amount of equal to or less than 80% by weight relative to the weight of the particulate product {e.g. from 1 % to 80%, from 10% to 80%, from 20% to 80%, from 30% to 80%, from 40% to 80%, from 50% to 80%, from 60% to 80%, or from 70% to 80% by weight). In a further embodiment, the liquid is present in an amount of equal to or less than 60% by weight relative to the weight of the particulate product (e.g. from 1 % to 60%, from 10% to 60%, from 20% to 60%, from 30% to 60%, from 40% to 60%, or from 50% to 60% by weight).

In an embodiment, the liquid is present in an amount of equal to or less than 1 .5 ml/g. In other words, for every 1 g of the particulate product, up to 1.5 ml of liquid may be loaded onto said particulate product. For example, the liquid may be present in an amount from 0.01 ml/g to 1 .5 ml/g, from 0.05 ml/g to 1 .5 ml/g, from 0.1 ml/g to 1 .5 ml/g, from 0.5 ml/g to 1 .5 ml/g, from 0.7 ml/g to 1.5 ml/g, from 0.9 ml/g to 1 .5 ml/g, from 1.0 ml/g to 1.5 ml/g, from 1 .1 ml/g to 1 .5 ml/g, from 1 .2 ml/g to 1 .5 ml/g, from 1.3 ml/g to 1 .5 ml/g, or from 1 .4 ml/g to 1.5 ml/g.

The formulation may be in the form of a powder. In the context of the present invention, the term "powder" can be defined in one of two ways; either as a loose grouping or aggregation of solid and/or hollow particles having a diameter smaller than about 1 mm, or as a dry, bulk solid composed of very fine particles having a diameter smaller than about 1 mm that is able to flow freely when shaken or tilted.

In preferred embodiments of the invention, the formulation is in the form of a free- flowing powder. The term "free-flowing powder" refers to a powder that has an angle of repose of 63° or less. In order to determine the angle of repose, the powder is sieved (mesh size 0.5 mm) onto a circular stainless steel support having a diameter of 50 mm so as to form a cone. Once the cone has reached its maximum height, the angle of repose is then calculated by taking the inverse tangent of the height of the cone in mm divided by half the width of the support. In an embodiment of the invention where the liquid is oil and the particulate product is a particulate salt product (e.g. a particulate sodium chloride or potassium chloride product), the formulation comprises oil in an amount between about 0.01 % to about 55% by weight relative to the total weight of the formulation. For example, the formulation may comprise oil in an amount of about 1 %, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 1 1 %, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21 %, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31 %, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41 %, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51 %, 52%, 53%, 54% or about 55% by weight relative to the total weight of the formulation.

The liquid may be one or more selected from the group consisting of an oil, a water-oil emulsion, a water-based liquid, propylene glycol, polypropylene glycol, glycerine or 1 , 3-propane diol. In the context of the present invention, the term oil(s) includes oily liquids.

Examples of water-based liquid that can be used in the present invention include, but are not limited to, a highly concentrated liquid with low water activity (e.g. less than 0.8), e.g. a flavouring component such as vegetable concentrate (e.g. onion) or yeast extract concentrate.

The water-based liquid may be a saturated solution of a salt (e.g. a saturated solution of sodium chloride or potassium chloride).

The water-based liquid may have a dry solids content of more than 20%, more than 30%, more than 40%, more than 50%, more than 60%, more than 70%, more than 75%, more than 80%, more than 85% or more than 90% by weight relative to the total weight of the liquid. For example, the water-based liquid may have a dry solids content of up to 90% by weight relative to the total weight of the liquid. For example, the water- based liquid may contain dry solids in an amount between 20% and 90%, 30% and 90%, 40% and 90%, 50% and 90%, 60% and 90%, 60% and 85%, 70% and 85% or 75% and 85% by weight relative to the total weight of the liquid. In embodiments in which the water-based liquid has a dry solids content of more than 20%by weight relative to the total weight of the liquid, the dry solids may contain a salt (e.g. sodium chloride or potassium chloride) in an amount from 2% to 100% by weight relative to the total weight of the dry solids content. The water-based liquids may form emulsions with oils. The resulting emulsions may be loaded onto the particulate products disclosed herein. In preferred embodiments of the present invention, the liquid is an oil.

Oils which may be contemplated in the context of the present invention include, but are not limited to essential oils, oleoresins, oil-based colourings, vegetable oils, animal fats or oils, vitamin oils and oily additives. In certain embodiments of the invention, the formulation may comprise more than one oil loaded on the particulate product. Preferably, the oil used in the preparation of the formulation is any oil or fat that is liquid or that can be liquefied at ambient conditions.

Examples of essential oils that can be used in the present invention include, but are not limited to, agar oil, ajwain oil, angelica root oil, anise oil, basil oil, bay oil, bergamot oil, carraway oil, cardamom seed oil, carrot seed oil, cedarwood oil, chamomile oil, cinnamon oil, citronella oil, clove leaf oil, coriander oil, cranberry seed oil, cumin oil, curry leaf oil, dill oil, eucalyptus oil, fennel seed oil, fenugreek oil, frankincense oil, galangal oil, garlic oil, geranium oil, ginger oil, grapefruit oil, henna oil, horseradish oil, jasmine oil, juniper berry oil, lavender oil, lemon oil, lemongrass oil, lime oil, mandarin oil, mint oil, mustard oil, neem oil, nutmeg oil, onion oil, oregano oil, parsley oil, peppermint oil, pine oil, rose oil, rosemary oil, sage oil, sandalwood oil, spearmint oil, tarragon oil, tea tree oil and thyme oil. Oleoresins are mixtures of a resin and an essential oil. Examples of oleoresins that can be used in the present invention include, but are not limited to, anise oleoresin, paprika oleoresin, black pepper oleoresin, capsaicin/capsicum, oleoresin, cardamom oleoresin, celery oleoresin, clove oleoresin, coriander oleoresin, cumin oleoresin, fennel oleoresin, fenugreek oleoresin, garlic oleoresin, ginger oleoresin, nutmeg oleoresin and onion oleoresin.

Oil-based food colourings that can be used in the present invention include, but are not limited to, carotenoids such as beta-carotene. Vegetable oils that can be used in the present invention include, but are not limited to, almond oil, coconut oil, corn oil, cottonseed oil, olive oil, palm oil, peanut oil, rapeseed oil, sesame oil, soybean oil, sunflower oil, beech nut oil, brazil nut oil, cashew oil, hazelnut oil, macadamia oil, pecan oil, pine nut oil, pistachio oil and walnut oil.

Animal fats or oils that can be used in the present invention include, but are not limited to tallow oil and fish oil (e.g. cod liver oil, mackerel oil, sardine oil and salmon oil). Therefore, the oil powder can be used as a means for delivering compounds with health benefits (e.g. omega-3 fatty acids) to patients in need thereof.

Vitamin oils that can be used in the present invention include, but are not limited to tocopherols such as a-tocopherol, β-tocopherol, γ-tocopherol and δ-tocopherol.

Oily additives that can be used in the present invention include, but are not limited to polysorbate (such as polysorbate 20, 40, 60 and 80) and mineral oil (e.g. paraffinic oil and naphthenic oil).

In embodiments of the present invention wherein the liquid is a water-oil emulsion, the above mentioned oils are contemplated in said emulsion.

The formulation may optionally include one or more further components selected from the group consisting of anti-caking agents, artificial colours, antioxidants, preservatives and the like. The formulation of the present invention is prepared by a process which comprises the step of blending a liquid (e.g. an oil, a water-oil emulsion, a water-based liquid, propylene glycol, polypropylene glycol, glycerine or 1 , 3-propane diol) with a particulate product comprised of particles that contain one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative) and an organic material that is a solid at ambient temperature. As already described herein, the particles have a structure comprised of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative (e.g. one or more of sodium chloride, potassium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative) attached together in the particles and at least some of the particles are hollow particles formed of an outer shell of said crystallites. In certain embodiments, a single type of liquid is blended with the particulate product. However, it is possible to load the particulate product with more than one type of liquid. Accordingly, other embodiments of the process include the step of blending more than one type of liquid with the particulate product.

As described above, at least some of the particles of the particulate product are hollow particles that can be termed "microspheres". As the microspheres are typically able to withstand blending, the step of blending the ingredients of the formulation may be performed using standard blending equipment that would be familiar to one skilled in the art. For example, a Lodige type plough blender may be used. However, care should be taken when blending using a high shear mixer with a knife to avoid breakage of the individual microspheres.

The liquid that is to be loaded onto the particulate product may be mixed with the particulate product prior to the blending step. However, it is preferred if the liquid is gradually dosed onto the particulate product during the blending step, for example, by spraying the liquid into the blender containing the particulate product. Alternatively, the liquid may be dosed onto the particulate product by dropwise addition. This gradual dosing improves the dispersal of the liquid onto the particulate product and shortens the time to homogeneity (i.e. production of the formulation).

In embodiments of the invention wherein the liquid is one or more of an oil, a water-oil emulsion, a water-based liquid, propylene glycol, polypropylene glycol, glycerine or 1 , 3-propane diol, solvents may be added to the liquid prior to blending or mixing with the particulate product. This can help to liquefy the liquid, which is particularly preferable if the liquid to be loaded onto the particulate product has a high viscosity. Liquefying the liquid prior to blending with the particulate product eases dispersal of the liquid with the particulate product and can prevent clumping of the particulate product during blending. There are no particular restrictions on the type of solvent that can be used to liquefy the liquid. However, if the formulation is for use in food then a food grade solvent should be used. In embodiments of the invention wherein the liquid is an oil, examples of solvents that may be added in order to liquefy the oil include, but are not limited to, medium chain triglycerides (which are triglycerides whose fatty acids have an aliphatic tail of from 6 to 12 carbon atoms) and alcohols (e.g. ethanol (96% v/v)).

If any excess solvent remains, it may be desirable to remove it prior to use of the formulation in final applications (e.g. in some food applications). Excess solvent may be removed under reduced pressure, for example.

Certain liquids such as oils may be sensitive to air oxidation during the blending process. In addition, air that becomes trapped in the formulation during the blending process may affect the stability of the oil during storage. Therefore, it may be preferable to blend the oil with the particulate product in the absence of air in cases where the oil is sensitive to air oxidation. For example, this could be achieved by performing the blending under vacuum. Alternatively, the blending may be performed in the presence of an inert atmosphere (e.g. an atmosphere of argon, nitrogen etc.). This also applies mutatis mutandis to other liquids that may be sensitive to air oxidation.

Typically, the blending of the liquid with the particulate product is performed at ambient (room) temperature. The fact that the formulation of the present invention can be produced at ambient temperature is advantageous because it avoids the need to heat the blending mixture (c.f. conventional spray-drying methods) which can increase the risk of thermal degradation of the liquid(s) to be loaded onto the particulate product. The blending may be performed at cooler temperatures (e.g. from about 5 °C to about 15 °C) if required to minimise the risk of air oxidation of the liquid (e.g. oil) during the blending process.

A significant use of the formulation of the present invention is as a seasoning for food.

In preferred embodiments of the present invention, the particulate product is a particulate sodium chloride product.

Conventional seasonings for food products (in particular, snacks) are typically powders that are made by blending different flavouring components, in powder or oily liquid form, with sodium chloride and carriers like maltodextrin. The sodium chloride is used to deliver the salty taste but also as a carrier of the (often oily) liquid flavouring components. The maltodextrin is also used as a carrier, however, it also has an additional role in that it provides bulk to the seasoning in order for it to have a larger volume/weight to homogenously cover the surface of the snack. By way of example, it is common to apply 50-60 g (and sometimes up to 80-100 g) of seasoning per 1 kg of potato chips.

The different flavouring components are selected and combined together to achieve desired flavour and taste characteristics. The components usually consist of a "core" flavour, which is often a concentrated oil-soluble liquid and gives the desired flavour note, and one or more taste enhancers, which bring the umami/kokumi taste and background and body notes in order to balance the taste of the more volatile components of the core flavour. By using formulations of the present invention in which the particulate product is a particulate sodium chloride or potassium chloride product as a seasoning instead of salt alone, less carrier is required than would otherwise be needed to carry the oil- soluble core flavouring components and to achieve the desired volume to homogeneously cover the surface of the snack. Accordingly, the present invention is advantageous in that it is possible to reduce the overall dosage of the seasoning (which has cost and health benefits) whilst at the same time improving the consistency of coverage of the snack.

Further, since embodiments of the formulation contain the particulate sodium chloride or potassium chloride product, the formulation is able to function as a carrier for multiple oils and provide saltiness at the same time in the final product. Accordingly, the formulation represents a new way to deliver flavours to food products.

As already discussed, in certain embodiments of the invention, the organic material used to bind the particles may be one or more of hydrolysed vegetable protein or yeast extract. Not only do these components serve to bind the particles together, but they are also taste enhancers that have strong secondary flavouring properties, and which could be used to enhance umami/kokumi taste. Accordingly, by loading selected oil-soluble core flavourings on these particulate products, it is possible to manufacture, in a cost efficient manner, a "stand-alone" seasoning (i.e. without the need for other flavouring components) having a well-balanced flavour note that is capable of homogeneously covering the surface of snacks. By varying the core flavour loaded onto the particulate product, a range of different seasonings with different flavour notes are readily envisaged.

Some seasonings are not provided in powder form, but in the form of an oily paste. Examples include savoury pastes made of spices, salt and large quantities of vegetable oil (e.g. more than 50% oil). The present invention can be used to modulate the texture of these pastes by replacing part of the salt with the particulate product and subsequently increasing the viscosity of the paste as a result of loading the vegetable oil onto the particulate product. The seasoning will have a different texture that enables the design of new products or easier handling which could reduce waste. On another hand, the ratio of expensive spices versus oil could be reduced in the seasoning recipe without affecting the texture, enabling cost reduction. Examples of such seasonings include, but are not limited to culinary seasonings (i.e. seasonings for cooking), seasonings for instant noodles and peanut butter spread.

In summary, the formulations of the present invention represent a new way to deliver flavours to food and beverage products when compared with standard seasonings. Furthermore, since the formulation is an effective delivery vehicle for oils, it has animal feed, cosmetic and industrial applications too.

If the formulation of the present invention is for use in food then the salt in the particulate salt product and the liquid (e.g. oil) should be of food grade quality.

As regards food applications, the formulation of the present invention may be used for the topical seasoning of food products (e.g. salads, soups etc.) by applying the formulation to the food product. For example, essential oils (e.g. basil and chili oil) can be loaded onto the particulate salt product and dosed as a final topping of a hot food product such as a pizza or pasta dish. The heat of the pizza or pasta dish, in combination with evaporating moisture, will melt the formulation of the present invention and liberate the full flavour and aroma of herbs and spices at the moment of consumption. When the formulation is intended to be used as a topical seasoning of a food product, it may be provided in the packaging of said food product for application thereto prior to consumption. For example, the formulation may be provided in the packaging in the form of a sachet. Alternatively, the formulation may be provided as a table-top seasoning.

Alternatively, the formulation of the present invention may be used as a semi-finished product, for example, a savoury building block to deliver savoury flavour and seasoning to food and drink products. When used as a savoury building block, the formulation of the present invention is typically mixed with other powdered seasoning or flavouring components (e.g. herbs and spices) to afford a powdered seasoning or flavouring that can be applied directly to food and beverage products.

The formulation of the present invention can also be used in a broad range of savoury applications, in particular, savoury dry semi-finished applications such as functional blends, compounded flavours, seasoning for snacks, table-top seasoning, and dry seasonings for instant noodles and diet foods.

It is also contemplated that the formulation of the present invention could be included in a dry product mix that requires reconstituting with liquid prior to consumption. Examples of such dry product mixes include dry soups and dry sauces, which are sold as such in the retail market, and which can be rehydrated with water (or other liquids such as milk) to make a soup or a sauce.

The formulation of the present invention may, if desired, be used as a blend with a "salty seasoning", the blend being intended for topical application to a relatively bland edible substrate (e.g. a cracker). Alternatively, the formulation may be incorporated in a precursor of a foodstuff (e.g. cake or bread mix) which is then cooked to produce the foodstuff. The formulation may also be added to sauces to impart seasoning and flavour. The formulation can also be used for any other food seasoning application.

Without limitation, the formulation may be used for seasoning meat products, fish products and bread products. Further, the formulation may be used to replace or reduce the amount of anti-caking additive added to savoury blends to keep them free flowing. Furthermore, since the formulation of the present invention is an effective delivery vehicle for liquids, in particular, oils, it has animal feed, cosmetic and industrial applications too. The formulation of the present invention can, for example, be used to introduce oils into cosmetic products. For example, the formulation may be incorporated into a cosmetic cream composition, a pressed powder cosmetic composition, a foundation, an eye shadow, a lipstick, a product having care properties, a mascara, an eyeliner, a concealer, or a product for making up the body.

The formulation of the present invention may also be incorporated into animal feeds. Advantageously, the formulation allows oil products (e.g. vitamins) to be carefully dosed into said animal feeds. The formulation of the present invention has industrial applications too. In particular, the formulation can be used as a safe way to dispose of hazardous liquids (e.g. hazardous oils). For example, in the event of an unwanted spillage of a hazardous liquid, the formulation can be spread over the affected area so as to convert the spilled liquid into an easy to dispose of powder. Accordingly, the formulations of the present invention have the ability to be used as cleaning/decontaminating agents.

As described above, the particulate product comprises at least a proportion of hollow particles comprised of an outer shell formed of individual crystallites of the one or more of sodium chloride, potassium chloride, calcium chloride, a phosphate, a carbonate, a sulfate and a cellulose derivative attached together to form the shell, which itself surrounds the hollow interior cavity of the particle. The following preparation examples describe how such hollow particles (microspheres) can be produced using the methods described herein. Preparation Example 1

The following aqueous solutions were prepared having a dry solids content of 25% by weight:

Solution 1) 2wt% malic acid and 98wt% sodium chloride on a dry solids basis.

Solution 2) 6wt% malic acid and 94wt% sodium chloride on a dry solids basis.

Solution 3) 2wt% malic acid and 98wt% potassium chloride on a dry solids basis. Solution 4) 6wt% malic acid and 94wt% potassium chloride on a dry solids basis.

The solutions were spray dried using a LabPlant™ lab scale spray dryer to produce Samples 1 to 4 (corresponding to solutions 1 to 4, respectively). All four samples were imaged using scanning electron microscopy (SEM). The images are shown in Figure 5. Sample 1 consisted of individual microspheres that were observed to be hollow as viewed in Figure 5. Samples 2-4 also consisted of hollow spheres.

Preparation Example 2

A 25% by weight dry solids aqueous solution consisting of 92.8wt% potassium chloride and 7.2wt% Gum Arabic on a dry solids basis was prepared. The solution was spray dried using the LabPlant™ lab scale spray dryer. The resultant hollow spheres were imaged by SEM and are shown in Figure 6.

Preparation Example 3

A 38% by weight dry solids aqueous solution consisting of 69.2wt% sodium chloride, 20.3wt% calcium chloride, and 10.5wt% gum arabic on a dry solids basis was prepared. The solution was spray dried using the LabPlant™ lab scale spray dryer. The resultant hollow spheres were imaged by SEM and are shown in Figure 7.

Preparation Example 4

A 38.2% by weight dry solids aqueous solution consisting of 68.8wt% sodium chloride, 20.2wt% calcium chloride, 10.5wt% gum arabic and 0.5wt% high nucleotide (HN) yeast extract on a dry solids basis was prepared. The solution was spray dried using the LabPlant™ lab scale spray dryer set. The resultant hollow spheres were imaged by SEM and are shown in Figure 8.

Preparation Example 5

A 38% by weight dry solids aqueous solution consisting of 93.8wt% hydrolyzed vegetable protein (HVP) lite (50% reduced sodium using potassium), and 6.2wt% gum arabic on a dry solids basis was prepared. The solution was spray dried using the LabPlant™ lab scale spray dryer. The resultant hollow spheres were imaged by SEM and are shown in Figure 9.

Preparation Example 6

A 30.2% by weight dry solids aqueous solution consisting of 92.9wt% sodium chloride, and 7.1wt% pullulan (PI20) on a dry solids basis was prepared. The solution was spray dried using the LabPlant™ lab scale spray dryer. The resultant hollow spheres were imaged by SEM and are shown in Figure 10.

Preparation Example 7

The following aqueous solutions were prepared:

Solution 1) 15wt% sodium bicarbonate and 1.5wt% Merigel™ (starch).

Solution 2) 15wt% sodium bicarbonate and 1.5wt% Mira-Mist® SE (Modified Starch). Solution 3) 15wt% sodium bicarbonate and 1.5wt% Promitor® L70 (Soluble gluco fibre).

Solution 4) 15wt% sodium bicarbonate and 1.5wt% Locust Bean Gum (Genu gum). Solution 5) 15wt% sodium bicarbonate and 1.5wt% Maltosweet™ 120 (Maltodextrin). Solution 6) 15wt% sodium bicarbonate and 1.5wt% low acyl gellan gum

(Kelcogel® F).

Solution 7) 15wt% sodium bicarbonate and 1.5wt% pullulan.

Solution 8) 15wt% sodium bicarbonate and 1.5wt% Pectin (Genu pectin).

Solution 9) 15wt% sodium bicarbonate and 1.5wt% Xanthan Gum (Keltrol® T). The solutions were spray dried using a Buchi Mini Spray Dryer B-290 to produce Samples 1 to 9 (corresponding to solutions 1 to 9, respectively). All nine samples were imaged using scanning electron microscopy (SEM). The images for Samples 1 to 9 are shown in Figures 11A to 111, respectively.

Examples

The invention will now be illustrated by means of the following examples, it being understood that these are intended to explain the invention, and in no way to limit its scope.

Example 1

This example compares the ability of oil to be loaded onto: (1) SODA-LO® Extra Fine M; (2) a particulate salt product (Salt Product A) comprised of particles which contain sodium chloride and acacia gum, and which have a structure comprised of individual crystallites of sodium chloride attached together in the particles of the product and wherein at least some of the particles of the product are hollow particles formed of an outer shell of said crystallites, wherein the particulate salt product has an average particle size by volume of 600 μηι and wherein at least about 90% by volume of the particles of the particulate salt product have a size less than about 1 100 μηι; and (3) regular salt.

10 g of SODA-LO® Extra Fine M (batch 022014, Tate & Lyle), Salt Product A (batch DL 13/90002, Tate & Lyle) and kitchen salt (Cerebos Esco France) were independently dry blended using a spoon with 0.1 g, 0.3 g, 0.5 g, 1.0 g, 3.0 g, 6.0 g and 10.0 g of sunflower oil (Maurel/Lesieur) to prepare blends containing 1 %, 3%, 5%, 10%, 30%, 60% and 100% by weight sunflower oil with respect to the total weight of the salt product used, respectively. The obtained blends (including a control salt product to which no oil had been added) were placed on a standard blue paper and left for one day at ambient temperature.

The outcome of the experiment is depicted in Figure 1. SODA-LO® Extra Fine M was able to absorb/adsorb the sunflower oil at higher loads compared to regular kitchen salt. Specifically, for SODA-LO® Extra Fine M, a much higher oil loading was achieved compared to regular kitchen salt (10 g oil onto 10 g SODA-LO® Extra Fine M).

Example 2

This example compares the ability of a coloured oil mixture to be loaded onto: (1) SODA-LO® Extra Fine M; (2) Salt Product A (see Example 1); and (3) regular salt. The coloured oil mixture contained 97 g of sunflower oil (Lesieur) and 3 g of Necol™ Orange #185779 paprika oleoresin (Synthite) per 100 g.

10 g of SODA-LO® Extra Fine M (batch 022014, Tate & Lyle), Salt Product A (batch DL 13/90002, Tate & Lyle) and kitchen salt (Cerebos Esco France) were independently dry blended using a spoon with 0.1 g, 0.3 g, 0.5 g, 1.0 g, 3.0 g, 6.0 g and 9.0 g of a coloured oil mixture to prepare blends containing 1 %, 3%, 5%, 10%, 30%, 60% and 90% by weight sunflower oil with respect to the total weight of the salt product used, respectively. The obtained blends (including a control salt product to which no oil had been added) were placed on white paper (80 g/m 2 , Business Class: Ref 58431) and left for one hour at ambient temperature. The outcome of the experiment is depicted in Figure 2. SODA-LO® Extra Fine M was able to absorb/adsorb the sunflower oil at higher loads compared to regular kitchen salt. Within 1 hour the oil loaded onto the regular kitchen salt began to be absorbed by the white paper at an oil loading of only 0.5 g per 10.0 g of salt. For SODA-LO® Extra Fine M, a 6 to 12 times higher oil loading could be achieved until a similar effect was observed. For Salt Product A, over 2 times higher oil loading could be achieved until a similar effect was observed.

Example 3 This example compares the oil loading of SODA-LO® Extra Fine M with regular kitchen salt in a centrifugation test.

Test tubes were filled with 3.0 g of sunflower oil (Lesieur) and 2.5 g of either regular kitchen salt (Cerebos Esco France) or SODA-LO® Extra Fine M (batch 022014, Tate & Lyle). Each test tube was subjected to centrifugation at 1000 g (g-force) for 5 minutes. Following centrifugation, no oil separation was observed for SODA-LO® Extra Fine M whereas clear oil separation was observed for regular kitchen salt (see Figures 3A and 3B). Accordingly, this experiment shows that a theoretical loading capacity of 120 g of oil per 100 g of particulate salt product can be achieved.

Example 4

Liquid pepper flavour was plated onto regular kitchen salt (Sel de table; Groupe Auchan France: Ref: EMB 54176) and 10 g of SODA-LO® Extra Fine M (batch 022014, Tate & Lyle) in a dosing of 15% by weight relative to the total weight of the loaded salt product (i.e. for every 100 g of loaded salt product, there is 15 g of pepper oil loaded onto 85 g of the salt product). The liquid pepper flavour was prepared by blending pepper oil, pepper oleoresin and capsicum oleoresin (all Synthite).

The 15% by weight dosage of the liquid pepper flavour turned the regular kitchen salt into a wet, clumpy, sticky and difficult to dose product (see Figure 4A and 4B). In contrast, SODA-LO® Extra Fine M loaded with liquid pepper flavour at an amount of 15% by weight was a powdery product that was easy to dose and easy to dilute for further usage. Accordingly, the loaded SODA-LO® Extra Fine M can be used as a concentrated intermediate for compounding savoury blends.




 
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