Login| Sign Up| Help| Contact|

Patent Searching and Data


Title:
PROCESS FOR MAKING AMORPHOUS POROUS PARTICLES FOR REDUCING SUGAR IN FOOD
Document Type and Number:
WIPO Patent Application WO/2018/100059
Kind Code:
A1
Abstract:
The present invention relates to process of making amorphous porous particles comprising sugar, a bulking agent and surfactant, having a closed porosity of at least 40% or between 20 and 60%. Further aspects of the invention relate to a food product comprising the amorphous porous particles; and a fat based confectionery product containing them; and the use of the amorphous porous particles as sugar replacers in food products such as fat based confectionery products for example, chocolate.

Inventors:
CURTIS PHILIP (CH)
DEDISSE ANNE-JULIETTE (CH)
DUPAS-LANGLET MARINA (CH)
GIANFRANCESCO ALESSANDRO (CH)
WHITEHOUSE ANDREW (GB)
Application Number:
PCT/EP2017/080964
Publication Date:
June 07, 2018
Filing Date:
November 30, 2017
Export Citation:
Click for automatic bibliography generation   Help
Assignee:
NESTEC SA (CH)
International Classes:
A23G1/40; A23G1/56; A23L27/00; A23L27/30; A23P10/20; A23P10/40; A23G9/34; A23G9/40
Foreign References:
US20160242432A12016-08-25
US20100215818A12010-08-26
US3746554A1973-07-17
Other References:
None
Attorney, Agent or Firm:
LUMSDEN, Stuart, Edward, Henry (CH)
Download PDF:
Claims:
Claims

1 . A process of making amorphous porous particles comprising the steps of;

a. subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, for example a pressure of 50 to 300 bars;

b. adding gas to the said mixture;

c. spraying and drying the said mixture to form agglomerated amorphous particles; and

d. deagglomerating the said particles to obtain amorphous porous particles having a reduced particle size.

2. A process according to claim 1 wherein said step c is carried out to obtain agglomerated amorphous porous particles having a D90 particle size of between 120 and 600 microns.

3. A process according to anyone of claims 2 wherein said step c is carried out to obtain agglomerated amorphous porous particles having a glass transition temperature of at least 40°C or higher.

4. A process according to claim 1 wherein said step d is carried out to obtain deagglomerated amorphous porous particles having a D90 particle size of between 100 to 200 microns.

5. A process according to claim 4 wherein said step d is carried out using high shear mixing or said step d is carried out using milling, for example hammer milling.

6. A process according to claim 5 wherein the high-shear mixing is carried out using a high-shear mixer, preferably wherein the high shear mixing is carried out at high speeds between 2000 and 4000 rpm.

7. A process according to claim 5 wherein the hammer milling is carried out at a speed of between 2000 and 7000 rpm, preferably wherein the hammer milling is carried out using a mesh size of between 0.1 and 0.4 mm.

8. A process according to any one of claims 5 to 7 wherein the deagglomeration of the amorphous porous particles is carried out using high shear mixing in a fat based matrix, preferably wherein the fat based matrix is for example vegetable oil or fat such as cocoa butter or chocolate, or liquefied chocolate.

9. A process according to any one of claims 1 to 8 wherein said step d is carried out to obtain amorphous porous particles, wherein said particles have a closed porosity of at least 40%.

10. A process according to claim 8 wherein milling is used to prepare the deagglomerated particles and the particles obtained have between 10 to 40% of non-spherical particles.

1 1 . A process according to any one of claims 1 to 10 wherein the gas is selected from the group consisting of nitrogen, carbon dioxide, air, argon and nitrous oxide.

12. A process according to claim 1 wherein the drying is spray-drying.

13. Amorphous porous particles obtainable according to the process described in steps a to c of claim 1.

14. Amorphous porous particles obtainable according to the process described in any one of claims 1 to 12.

15. A food product comprising the amorphous porous particles according to claim 14, preferably where said food product is a fat based confectionery product, for example chocolate.

16. Use of the amorphous porous particles according to claim 14 as a sugar replacer in a food product.

Description:
PROCESS FOR MAKING AMORPHOUS POROUS PARTICLES FOR REDUCING SUGAR IN FOOD

Field of the invention

The present invention relates to a process for making a low sugar composition. In particular the invention relates to a process of making amorphous porous particles comprising sugar, a bulking agent and surfactant, having a closed porosity .The invention also relates to a food product comprising the amorphous porous particles; and the use of the amorphous porous particles as sugar replacers in food products particularly confectionery products such as for example, chocolate.

Background of the invention Any discussion of the prior art throughout the specification should in no way be considered as an admission that such prior art is widely known or forms part of common general knowledge in the field.

The increasing interest in reduced sugar intake in the diet by health conscious consumers has led to a strong demand for food products with lower sugars. Sugar, however, is a key food ingredient that in addition to imparting natural sweetness to food products also functions to provide bulk and therefore plays a significant role in the structure, volume and mouthfeel of the finished food product.

Sugar is a naturally occurring sweetener that as aforementioned provides the sweetness in food products that consumers crave but is also highly calorific and so there is an important need for healthier, non-caloric or low-caloric sweetener alternatives. There have been many approaches that are well known in the art, involving the replacement or reduction of sugars in food products such as for instance using artificial sweeteners to replace natural sugar. More particularly, for example, for fat based confectionery products such as chocolate, many attempts have been made to provide a substitute for sugar using reduced sugar alcohols or 'polyols. Other approaches have included using bulking agents such as, non or low-caloric fibres to replace sugar in chocolate compositions. These approaches however, have associated disadvantages, for instance, polyols are well known to have undesirable laxative effects and furthermore such artificial sweeteners are not well perceived by consumers who have a preference for clean label products. There are also certain disadvantages linked to the use of bulking agents to replace sugars in food products this is mainly the associated undesirable impact on sweetness usually a reduction in sweetness. l Thus, it is generally well known to those skilled in the art of food manufacturing that replacing or reducing sugar in a food composition usually negatively impacts the flavour, and other taste components. For instance, sugar replacers may be slower in onset of the sweetness perception and longer in duration compared to natural sugar and so therefore change the taste balance of a food composition.

In addition, sugar replacers may not deliver as sweet a taste as natural sugar and may also exhibit, metallic, cooling, astringent, liquorice-like, and bitter after tastes.

In a further example, applying the prior art solutions as aforementioned for fat based confectionery products may also result in similar disadvantages. For instance, using bulking agents such as fibres in chocolate compositions leads to bitter aftertastes and adds undesirable bulk to the mixture, resulting in an increase in the viscosity of the mixture. This in turn makes it difficult to carry out the standard post-processing of the mixture such as enrobing and moulding which are essential steps towards furnishing a finished chocolate product. There thus remains the problem of providing low calorie or reduced sugar alternatives to natural sugar which may be used in food products or confectionery products without having a detrimental impact on the sweetness perception and/or any of the above associated problems of the prior art solutions.

Accordingly, there remains a need to find low calorie sugar replacers that can be used in a food product or confectionery compositions such as chocolate for example, which avoids the problems of loss or reduction in sweetness, bitter aftertastes and off-flavours.

Accordingly, there remains a need to provide low calorie sugar replacers that are "clean label" and more desirable to the consumer.

It is thus desirable to provide a healthier, reduced calorie or reduced or low sugar alternative to natural sugar that may be used in food products or confectionery products wherein there is little or no negative impact on sweetness perception.

In particular, there is a need to provide low sugar alternatives that may be easily industrialised at a reasonable cost.

More particularly, there is a need to be able to address for example the viscosity issues that are common when replacing sugar with alternative low sugar or low calorie bulking agents. There thus exists a need to solve one or more of the above mentioned problems.

It is an object of the present invention to ameliorate at least one disadvantage of the prior art as aforementioned of previous reduced or low calorie sugar alternatives such as artificial sweeteners and/or bulk sugar replacers such as fibres.

Summary of the invention Accordingly, this need is solved by the features of the independent claims. The dependent claims further develop the central idea of the invention.

Thus, in a first aspect, the present invention relates to a process of making amorphous porous particles comprising the steps of; subjecting a mixture comprising sugar, bulking agent and surfactant to a pressure of 50 to 300 bars; adding gas to the said mixture; spraying and drying the said mixture to form agglomerated amorphous particles; and deagglomerating the said particles to obtain amorphous porous particles having a reduced particle size. In one embodiment there is provided a process of the present invention wherein the deagglomeration is carried out by subjecting the agglomerated amorphous particles to high shear mixing.

In one embodiment there is provided a process of the present invention wherein the deagglomeration is carried out by milling for example hammer milling. In a further embodiment there is provided a process of the present invention wherein the deagglomeration of the amorphous porous particles may be carried out in fat based matrix for example vegetable oil or cocoa butter or liquefied chocolate or chocolate mass

Preferably, the agglomerated amorphous porous particles of the invention are preferably mixed with fat, for example, any oil such as vegetable oil, cocoa butter or liquefied chocolate or chocolate

In a further embodiment there is provided a process of the present invention wherein the sugar is selected from the group consisting of sucrose, fructose, glucose, dextrose, galactose, allulose, maltose, high dextrose equivalent hydrolysed starch syrup xylose, and any combinations thereof

In a further embodiment there is provided a process of the present invention wherein the bulking agent is selected from the group consisting of maltodextrins, milk powder (for example skimmed milk powder (SMP)), whey powder (for example demineralised whey powder (DWP), soluble wheat or corn dextrin (for example Nutriose®), polydextrose, soluble fibre such as Promitor® and any combinations thereof.

In a further embodiment there is provided a process of the present invention wherein the surfactant is selected from the group consisting of sodium caseinate, lecithin and any combinations thereof

In another aspect of the present invention there is provided a process of making the amorphous porous particles comprising the steps of; subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar adding gas to the pressurised mixture; spraying and drying the mixture to form amorphous porous particles; and reducing the particle size of the amorphous porous particles.

In one embodiment, there is provided a process of the present invention wherein reducing the particle size of the amorphous porous particles is carried out by subjecting the agglomerated amorphous particles to high shear mixing, for example subjecting the agglomerated amorphous particles to high shear mixing or milling, for example, by hammer milling, such that they are deagglomerated.

In a further embodiment there is provided a process of the present invention wherein reducing the particle size of the amorphous porous particles (for example deagglomerating them) may be carried out in fat based matrix for example vegetable oil or cocoa butter or liquefied chocolate or chocolate. Preferably, the agglomerated amorphous porous particles of the invention are mixed with fat, for example, any oil such as vegetable oil, cocoa butter or liquefied chocolate or chocolate mass

In another aspect there is provided amorphous porous particles obtainable according to the process of the present invention In a further embodiment of the invention there is provided amorphous porous particles or deagglomerated amorphous porous particles comprising sugar, a bulking agent and a surfactant wherein said amorphous porous particles have a closed porosity of at least 40%.

In an additional embodiment of the invention there is provided amorphous porous particles or deagglomerated amorphous porous particles comprising sugar, a bulking agent and a surfactant wherein said amorphous porous particles have a closed porosity of at least 40%, and wherein between 10 to 40% of said particles are not round particles or non-spherical particles.

In a further embodiment there is provided deagglomerated amorphous porous particles of the present invention having a D90 particle size of between 100 and 200 microns, wherein said particles have a closed porosity of at least 40%, and wherein between 10 to 40% of said particles are 'not round' particles or non-spherical particles.

In a further embodiment of the invention there is provided amorphous porous particles or deagglomerated amorphous porous particles comprising sugar, a bulking agent and a surfactant wherein said amorphous porous particles have a closed porosity of between 20 and 60%.

In a further embodiment there is provided deagglomerated amorphous porous particles of the present invention having a D90 particle size of between 100 and 200 microns, wherein said particles have a closed porosity of at least 40% or between 20 and 60%.

In another embodiment of the invention there is provided a process of making agglomerated amorphous porous particles of the present invention having a closed porosity of at least 40% or between 20 and 60%. In one further embodiment of the invention there is provided a process of making agglomerated amorphous porous particles having a D90 particle size of between 120 and 600 microns.

In an additional embodiment, there is provided a process of making deagglomerated amorphous porous particles of the present invention having a D90 particle size of between 100 and 200 microns.

In a further embodiment there is provided deagglomerated amorphous porous particles of the present invention having a D90 particle size of between 100 and 200 microns, wherein said particles have a closed porosity of at least 40% or between 20 and 60%.

In an additional embodiment there is provided agglomerated amorphous porous particles of the present invention having a D90 particle size of between 120 and 600 microns, wherein said particles have a closed porosity of between 20 to 60%.

In an additional embodiment there is provided a process according to the present invention wherein the deagglomerated particles obtained have between 10 to 40% of said particles that are non-spherical particles.

In a further embodiment there is provided deagglomerated amorphous porous particles of the present invention having a D90 particle size of between 100 and 200 microns, wherein said particles have a closed porosity of at least 40%, and wherein between 10 to 40% of said particles are non-spherical particles.

It has been surprisingly found by the inventors that the amorphous porous particles of the present invention can be used to replace sugar (such as sucrose) in a food product for example without having a detrimental effect on the sweetness of the food product.

Also advantageously, it was found that the agglomerated amorphous porous particles of the present invention overcome the problems normally associated with handling amorphous sugar based powder materials and can, contrary to known amorphous sugar based materials, be used in chocolate compositions, for example. Thus, due to the hygroscopic nature and so its water content amorphous sugar is not typically used in chocolate compositions. It undesirably absorbs water from the environment and other chocolate ingredients generating potential difficulties during processing and storage. Furthermore, the amorphous state can be unstable, and amorphous sugars, such as sucrose or dextrose, tend to rapidly crystallise in the presence of moisture and/or release moisture from crystallisation. Agglomerating particles leads to a smaller external surface area than the total external surface of the particles which formed the agglomerate. This means that they absorb water more slowly. Accordingly, the agglomerated particles of the present invention advantageously exhibit improved stability against moisture.

Advantageously, it was surprisingly found that at equivalent volumes the aerated amorphous porous particles of the present invention gave at least equivalent or more sweetness compared to a fuller denser crystalline sugar.

In another aspect, there is provided a food product comprising the amorphous porous particles of the present invention. The food product may for example contain 5 to 60 % of the amorphous porous particles. In a further aspect a food product according to the present invention is a confectionery product, a culinary product, a dairy product, a nutritional formula, a breakfast cereal or an ice-cream.

In a still further aspect of the present invention the food product is a fat based confectionery product for example chocolate.

In another aspect there is provided a use of the amorphous porous particles of the present invention as a sugar replacer in a food product. In a further aspect there is provided a use of the amorphous porous particles of the present invention to reduce the sugar content of a food product

Advantageously the present invention makes possible the preparation of food products such as fat based confectionery products in which the high calorific natural sugar can be wholly and/or partially replaced by the low calorific amorphous porous particles of the present invention.

In another aspect there is provided a use of the amorphous porous sucrose particles of the present invention as a sugar replacer in a food product.

It was surprisingly found that from between up to 30%, preferably 65%, more preferably, up to 70% of the usually required sweetener such as sugar can be eliminated from the foodstuff while still achieving the same desired level of sweetness perception using the amorphous porous particles of the present invention to replace.

In another aspect of the present invention there is provided a fat based confectionery composition comprising a) cocoa powder or cocoa liquor or cocoa butter or cocoa butter equivalents or any combinations thereof and b) 5 to 60 wt% of amorphous porous particles according to the present invention wherein said amorphous porous particles comprise sugar, a bulking agent and a surfactant, and wherein said amorphous porous particles have a closed porosity of at least 40% or between 20 and 60%.

In another aspect of the present invention there is provided a fat based confectionery composition comprising a) cocoa powder or cocoa liquor or cocoa butter or cocoa butter equivalents or any combinations thereof and b) 5 to 60 wt% of amorphous porous particles according to the present invention wherein said amorphous porous particles comprise sugar, a bulking agent and a surfactant, and wherein said amorphous porous particles have a closed porosity of at least 40% and wherein between 10 to 40% of said particles are not round particles or non-spherical particles.

In a further aspect, there is provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention, comprising the steps of;

subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar; adding gas to the mixture; spraying and drying the mixture to form agglomerated amorphous porous particles; mixing ingredients selected from the group consisting of milk powder, fat, cocoa liquor, crystalline sugar, lecithin and any combinations of these; refining the resulting mixture; liquefying the resulting refined mixture with further fat, and optionally lecithin reducing the particle size of the amorphous porous particles; and then

Adding the particle-sized reduced amorphous porous particles to the refined mixture before or after liquefying.

In another aspect there is provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention, comprising the steps of;

subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar; adding gas to the mixture; spraying and drying the mixture to form agglomerated amorphous porous particles; reducing the particle size of the amorphous porous particles; mixing ingredients selected from the group consisting of milk powder, fat, cocoa liquor, crystalline sugar, lecithin and any combinations of these; refining the resulting mixture; and liquefying the resulting refined mixture with further fat, the reduced particle size amorphous porous particles and optionally lecithin.

The liquefaction may for example be performed by conching. The fat may for example be cocoa butter, cocoa butter equivalent or cocoa butter replacer.

In a further embodiment there is a provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention wherein the said amorphous porous particles are reduced in particle size by hammer-milling, for example the said amorphous porous particles are deagglomerated by hammer-milling.

In a further aspect there is provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention, comprising the steps of;

subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar; adding gas to the mixture; spraying and drying the mixture to form agglomerated amorphous porous particles; deagglomerating the amorphous porous particles; mixing ingredients selected from the group consisting of milk powder, fat, cocoa liquor, crystalline sugar, lecithin and any combinations of these; refining the resulting mixture; and liquefying the resulting refined mixture with further fat, the reduced particle size amorphous porous particles and optionally lecithin. In a further embodiment there is provided a process of the present invention wherein reducing the particle size of the amorphous porous particles (for example deagglomerating the amorphous porous particles) may be carried out in fat based matrix for example vegetable oil or cocoa butter or liquefied chocolate or chocolate.

Preferably, the agglomerated amorphous porous particles of the invention are mixed with fat before being reduced in particle size, the fat may for example be any oil such as vegetable oil, cocoa butter or liquefied chocolate to chocolate.

The liquefaction may for example be performed by conching. The fat may for example be cocoa butter, cocoa butter equivalent or cocoa butter replacer.

In a further embodiment there is a provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention wherein the said amorphous porous particles are reduced in particle size by high shear mixing

The deagglomeration of the amorphous porous particles of the present invention may also be subjected to direct high shear mixing.

In another embodiment the reduced particle size amorphous porous particles may be added after the refining step and before the liquefaction step

In another aspect there is provided a use of the amorphous porous particles of the present invention as a bulk sugar replacer in a food product.

In a further aspect of the present invention, the food product is confectionery product, a culinary product, a dairy product, a nutritional formula, a breakfast cereal or an ice-cream.

In another aspect of the present invention there is provided a sugar replacement or sweetener composition comprising amorphous porous particles comprising sugar, a bulking agent and a surfactant, wherein said amorphous porous particles have a closed porosity of at least 40% or between 20 and 60%.

In another aspect of the present invention there is provided a sugar replacement or sweetener composition comprising amorphous porous particles comprising sugar, a bulking agent and a surfactant, wherein said amorphous porous particles have a closed porosity of at least 40% or between 20 and 60%,

In another aspect of the present invention there is provided a sugar replacement or sweetener composition comprising amorphous porous particles comprising sugar, a bulking agent and a surfactant, wherein said amorphous porous particles have a closed porosity of at least 40%.

In another aspect of the present invention there is provided a sugar replacement or sweetener composition comprising amorphous porous particles comprising sugar, a bulking agent and a surfactant, wherein said amorphous porous particles have a closed porosity of at least 40% and wherein and wherein between 10 to 40% of said particles are not round particles or non-spherical particles

In another aspect of the present invention there is provided a sugar replacement or sweetener composition comprising amorphous porous particles comprising sugar, a bulking agent and a surfactant, wherein said amorphous porous particles have a closed porosity of at least 40%, and wherein between 10 to 40% of said particles are not round particles or non-spherical particles

Surprisingly the amorphous porous particles of the present invention overcome the usual problems associated with handling amorphous powders such as hygroscopicity. Advantageously, the amorphous porous particles of the present invention are more stable and less likely to recrystallize to the lesser desirable crystalline form.

Furthermore, advantageously, the present invention makes possible the preparation of food products, in particular fat based confectionery food products incorporating the amorphous porous particles of the present invention, having better stability such as lesser likelihood of undesirable recrystallization of the sugar and so resulting in a longer shelf life of such products.

Advantageously the amorphous porous particles of the present invention are much easier to process in food recipes, for example chocolate recipes compared to conventional sugar. Further, advantageously the process of high shear mixing reduces the viscosity issues typically associated with agglomerated powders having large particle sizes.

Advantageously the aerated or porous structure of the amorphous porous particles of the present invention retain their structural integrity (for example their closed porosity) even when undergoing heavy processing for example conching during chocolate manufacture.

Furthermore, surprisingly the internal or closed porosity of the amorphous porous particles of the present invention retain their structural integrity and thus closed porosity even after harsh treatment with high shear mixer or even after harsh milling by treatment with hammer-milling. It has been surprisingly found by the inventors that the majority of the internal closed porosity of the amorphous porous particles of the present invention survives, more particularly that the particles retain at least 40 % or at between 20 and 60 % closed porosity after a deagglomeration process of aggressive treatment of high shear mixing

It has been surprisingly found by the inventors that the majority of the internal closed porosity of the amorphous porous particles of the present invention survives, more particularly that the particles retain at least 40 % closed porosity after a deagglomeration process by the harsh conditions of hammer -milling.

More surprisingly, the deagglomerated amorphous porous particles of the present invention even though largely fragmented and having larger D90 particle sizes still provided acceptable levels of porosity and sweetness when incorporated into fat based confectionery, for example chocolate.

Without being bound by theory, it is believed that particles comprising sugar in the amorphous state and having porosity (particularly internal closed porosity) provide a material which dissolves more rapidly than crystalline sugar particles of a similar size. This rapid dissolution in the oral cavity when consumed leads to an enhanced sweetness perception and ensures that more of the sugar is dissolved and reaches the tongue rather than being swallowed untasted.

In a further aspect of the present invention there is provided a sugar replacement composition suitable for partial or whole replacement of sugar in foodstuffs. Advantageously, the present invention provides replacement of sugar in foodstuffs but still achieving the same or similar level of sweetness. The present invention makes it possible to completely replace sugar in a foodstuff, for example a chocolate product, with the amorphous porous particles of the present invention, achieving at least 65% sugar reduction in one aspect of the present invention. Advantageously the amorphous porous particles of the present invention can be used as a natural low calorie sugar alternative. Thus, the amorphous porous particles of the present invention provide the reduction of sugar in food products without the need to use artificial sweeteners and/or conventionally known bulking agents.

Brief description of the drawings Additional features and advantages of the present invention are described in, and will be apparent from, the description of the presently preferred embodiments, which are set out below with reference to the drawings in which:

Figures 1a, 1 b, 1c are cryo-scanning electron microscopy images representing the microstructure of a conventional fat based confectionery composition magnified 500 times, 1000 times and 2000 times respectively. Milk powder particles are indicated at (1 ), Sucrose crystals at (2), and cocoa butter solids at (3).

Fig 2a shows a cryo-scanning electron microscopy image of non-agglomerated amorphous porous particles made according to Example 3

Fig 2b shows a cryo-scanning electron microscopy image of agglomerated amorphous porous particles made according to the present invention.

Fig 2c, shows an optical micrograph of the agglomerated amorphous porous particles of the present invention having been dispersed in MCT oil and viewed under transmitted light

Fig 2d show an optical micrograph of the amorphous porous particles deagglomerated by treating with high-shear mixing in cocoa butter Fig 2e shows an optical micrograph of the amorphous porous particles deagglomerated by subjecting to high shear mixing in liquefied chocolate

Figure 3 is a plot of glass transition temperature (Tg/ °C) versus sucrose content for amorphous porous particles of sucrose and skimmed milk powder at 25 °C and a water activity of 0.1 . Figure 4a, 4b, 4c, 4d are synchrotron radiation X-ray tomographic microscopy images for amorphous powders.

Figs 5a, 5b show a cryo-scanning electron microscopy images of deagglomerated amorphous particles made according to the present invention, magnified 2000 times and 1000 times respectively. The images show more fragmentation of the said particles after deagglomeration by hammer-milling, but even so substantial structural integrity of the internal or closed porosity can be clearly seen.

Detailed description of the invention and the preferred embodiments

According to the present invention, the term 'non-agglomerated' as used herein is to be understood in conventional terms and refers to the primary particle of the amorphous porous particles of the present invention. Figure 2a demonstrates the non-agglomerated amorphous porous particles as made under Example 3. The terms non-agglomerated or primary particles are used interchangeably. The desired primary particle size D90 is preferably between 50 and 100 microns.

According to the present invention the term 'agglomerated' as used herein is to be understood in conventional terms and refers to the primary particles associated together due to inter-particle forces. Agglomerates may consist of primary particles that are weakly bound together at their points of contact. These agglomerates contain multiple primary particles resulting in agglomerated masses with particles sizes many times larger than the size of the primary or non-agglomerated particles. In the context of the present invention the agglomerates formed according to the methods of the present invention have preferably a particle size D90 of between 120 and 600 microns.

The term "deagglomerated particles" as used herein is to be understood in conventional terms and refers to the agglomerated particles of the present invention that have been subjected to deagglomeration in accordance with the high shear process as described in the present invention. The impact of such deagglomeration leads to smaller chain of agglomerated masses or fragments or fractions or broken pieces. All terms as herein defined may be used interchangeably. Deagglomerated fractions are generally significantly smaller than the size of the parent agglomerated particles from which the fractions originate, and can range all the way down to primary particle size, depending upon the amount of mechanical energy imparted to the agglomerated particles.

According to the present invention the term 'amorphous' as used herein is defined as being essentially free of crystalline material and should be interpreted in line with conventional understanding of the term.

According to the present invention, the term glass transition temperature (Tg) as used herein is to be interpreted as is commonly understood, as the temperature at which an amorphous solid becomes soft upon heating or brittle upon cooling. The glass transition temperature is always lower than the melting temperature (Tm) of the crystalline state of the material. An amorphous material can therefore be conventionally characterised by a glass transition temperature, denoted Tg. Several techniques can be used to measure the glass transition temperature and any available or appropriate technique can be used, including differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA)

In a preferred embodiment of the present invention the amorphous porous particles are characterised as having a glass transition temperature of at least 40°C or higher, preferably at least 50°C or higher and more preferably at least 60°C or higher.

Advantageously in contrast to prior art solutions, the amorphous porous particles of the present invention are less hygroscopic making such material easier to handle and incorporate into conventional preparations of foodstuffs such as for example chocolate manufacture. According to the present invention, the term porous as used herein is defined as multiple non-interconnected small pores or voids or interstices that allow air or liquid to pass through. In the context of the present invention porous is also used to describe the aerated nature of the amorphous particles of the present invention.

In the present invention the term porosity as used herein is defined as a measure of the empty spaces (or voids or pores) in a material and is a ratio of the volume of voids to total volume of the mass of the material between 0 and 1 , or as a percentage between 0 and 100%

Porosity can be measured by means known in the art. For instance, the particle porosity can be measured by the following equation: Porosity= Vp-Vcm/Vp x 100 wherein Vp is the Volume of the particle and Vcm is the volume of the matrix or bulk material.

According to the present invention the term closed or internal porosity as used herein refers in general terms to the total amount of void or space that is trapped within the solid. As can be seen in the figures, fragmented or broken amorphous porous particles of the present invention show the internal microstructure wherein the voids or pores are not connected to the outside surface of the said particles. In the present invention the term closed porosity is further defined as the ratio of the volume of closed voids or pores to the particle volume.

It is known that increasing the porosity of the amorphous particles increases their dissolution speed in water. This increased dissolution speed enhances the sweetness impact of the particles. However, increasing the porosity of the particles also increases their fragility. It is advantageous that the porous amorphous particles of the present invention exhibit closed porosity. Particles with closed porosity, especially those with many small spherical pores, are more robust than particles with open pores, as the spherical shapes with complete walls distribute any applied load evenly. When added to a fat-based confectionery material, closed porosity has a further advantage over open porosity in that fat does not penetrate inside the particle. This penetration inside the particles would reduce the "free" fat available to coat all the particles in the fat-based confectionery material and lead to an increase in viscosity.

In a preferred embodiment of the present invention, the agglomerated amorphous porous particles have a closed porosity of between 15 to 80%, preferably 20 to 70%, more preferably 20 to 60%. In a further preferred embodiment, the agglomerated amorphous porous particles of the present invention have a closed porosity of between 40 to 60%, more preferably 50 to 60%.

In a preferred embodiment of the present invention, the deagglomerated amorphous porous particles have a closed porosity of at least 20%, preferably at least 30%, more preferably at least 40% and even more preferably at least 50% or between 20 and 60%. According to the present invention, the term density as used herein is defined in conventional terms as the volumetric mass density of a substance and this is the mass per unit volume of a material. Density should be interpreted in line with conventional understanding of the term.

In the context of the present invention, the term Bulk density as used herein refers to in conventional terms the weight of a unit volume of a loose material such as powder, to the same volume of water, and is typically expressed as kilograms per cubic metre (kg/cm 3 ) or g/cm 3

In a preferred embodiment of the present invention, the amorphous porous particles of the present invention have a density of between 0.3 to 1 .5 g/cm 3 , preferably 0.5 to 1 .0 g/cm 3 , more preferably 0.6 to 0.9 g/cm 3 .

According to the present invention, the term sphericity as used herein refers to in conventional terms a measure of how spherical (round) an object is. In the context of the present invention sphericity refer to the sphericity of the particles and is defined as

Sphericity = 4πΑ/Ρ 2 wherein A is defined as the measured area covered by a particle projection and P is the measured perimeter of a particle projection. For instance, an ideal sphere would have an expected the sphericity of 1 . The agglomerated porous particles of the present invention are made up of long chains of smaller primary particles of the said amorphous porous particles.

In an additional embodiment there is provided a process according to the present invention wherein the deagglomerated particles obtained have between 10 to 40%, preferably 15 to 35% of said particles that are not round particles or non-spherical particles

In a preferred embodiment, the deagglomerated amorphous porous particles have at least 70%, preferably at least 60% and more preferably at least 50% of said particles that are not round or non-spherical.

In a preferred embodiment of the present invention the deagglomerated amorphous porous particles have between 10 to 40%, more preferably 15 to 35% of said particles that are not round or non-spherical particles

In a preferred embodiment there is provided a process according to the present invention wherein the deagglomerated particles obtained have at least 70%, preferably at least 60% and more preferably at least 50% of said particles that are not round or non-spherical. In a preferred embodiment there is provided a process according to the present invention wherein the deagglomerated particles obtained have between 10 to 40%, more preferably 15 to 35% of said particles that are not round particles or non-spherical particles

According to the present invention there is provided a process of deagglomerating the dry amorphous porous powder material of the present invention otherwise known in the art as dry agglomeration.

The deagglomerated amorphous porous particles of the present invention have sphericity less than 0.9, preferably less than 0.8. The deagglomerated particles may have less than 70% of their surface being convex, for example less than 50%, for further example less than 25%. The agglomerated particles of the present invention are not spherical as can been seen in figure 2c. Furthermore the deagglomerated particles of the present invention are not spherical as can been seen in figures 2d and 2e.

According to the present invention there is provided a process of deagglomerating wet powder material for example the said amorphous porous particles are mixed with fat (for example fat comprised within chocolate) before deagglomeration otherwise known in the art as wet agglomeration. In the context of the present invention, the term fat refers to triglycerides. Fats are the chief component of animal adipose tissue and many plant seeds. Fats which are generally encountered in their liquid form are commonly referred to as oils. In the present invention, the terms oils and fats are interchangeable.

The deagglomerated amorphous porous particles of the present invention have sphericity less than 0.9, preferably less than 0.8. The deagglomerated particles may have less than 70% of their surface being convex, for example less than 50%, for further example less than 25%.

As previously described, the amorphous and porous nature of the particles leads to faster dissolution in the mouth. This not only enhances sweetness impact but is believed to make the particles less easily detected by the tongue and palate. Advantageously the highly porous and amorphous nature of the particles of the present invention provides an enhanced sweetness and attractive mouthfeel, particularly in fat based confectionery products where the prior art disadvantages associated with replacing sugar with conventional bulking agents usually leads to poor organoleptic qualities, such as grittiness and lack of sweetness. According to the present invention, the term particle size as used herein is defined as D90. The D90 value is a common method of describing a particle size distribution. The D90 is the diameter where 90 % of the mass of the particles in the sample have a diameter below that value. In the context of the present invention, the D90 by mass is equivalent to the D90 by volume. The D90 value may be measured for example by a laser light scattering particle size analyser.

In a preferred embodiment, the agglomerated amorphous porous particles of the present invention have a D90 particle size of between preferably 120 and 600 microns, preferably 150 and 600 microns, even more preferably 200 and 600 microns.

In one further embodiment of the invention there is provided a process of making agglomerated amorphous porous particles having a D90 particle size of between preferably 120 and 600 microns, preferably 150 and 600 microns, even more preferably 200 and 600 microns.

In a preferred embodiment, the deagglomerated amorphous porous particles have a D90 particle size of between preferably 100 and 200 microns, more preferably 1 10 and 170 microns and even more preferably 1 10 and 160 microns.

In an additional embodiment, there is provided a process of making deagglomerated amorphous porous particles of the present invention having a D90 particle size of between preferably 100 and 200 microns, more preferably 1 10 and 170 microns and even more preferably 1 10 and 160 microns.

In the present specification. All percentages are expressed by weight (wt%) unless otherwise specified. According to the present invention the term sugar as used herein refers to as is conventionally understood a sweet crystalline substance obtained from various plants, especially sugar cane and sugar beet, and used as a sweetener in food and drink. In the context of the present invention sugar is defined as and includes all mono, di and oligosaccharides for example sucrose, fructose, glucose, dextrose, galactose, allulose, maltose, high dextrose equivalent hydrolysed starch syrup, xylose, and combinations thereof. Accordingly, the sugar comprised within the amorphous porous particles according to the invention may be selected from the group consisting of sucrose, fructose, glucose, dextrose, galactose, allulose, maltose, high dextrose equivalent hydrolysed starch syrup xylose, and any combinations thereof. In a preferred embodiment, the amorphous porous particles of the present invention comprise sugar in the amount of 5 to 70%, preferably 10 to 50%, even more preferably 20 to 40%.

In one preferred embodiment, the amorphous porous particles of this invention comprise at least 70% sugar. According to the present invention the term bulking agent as used herein refers to as is conventionally understood a food additive that increases food volume or weight without impacting the utility or functionality of a food. In a particularly preferred embodiment of the present invention, the bulking agents of the present invention are low or non-calorific additives which impart bulk and provide advantageously healthier alternatives to for example sugar.

According to conventional understanding bulking agents may be used to partially or completely replace high-caloric ingredients, such as sugar so as to prepare an edible formulation with a reduction in calories. Additionally, the bulking agents are useful as a source of soluble fibre to be incorporated into foods and, unlike sugar, are non-cariogenic. In a preferred embodiment, the amorphous porous particles of the present invention comprise a bulking agent in the amount of 5 to 70%, preferably 10 to 40%, more preferably 10 to 30%

In one preferred embodiment, the amorphous porous particles of the present invention comprise preferentially 10 to 25% of the bulking agent. According to the present invention the bulking agent may be selected from the group consisting of polyols (sugar alcohols for example isomalt, sorbitol maltitol, mannitol, xylitol, erythritol and hydrogenated starch hydrolysates) guar gum, psyllium husk, carnuba wax, glycerin, beta glucan, polysaccharides (such as starch or pectin for example), dietary fibres (including both insoluble and soluble fibres) , polydextrose, methylcellulose, maltodextrins, inulin, milk powder (for example skimmed milk powder), whey, demineralised whey powder, dextrins such as soluble wheat or corn dextrin (for example Nutriose®), soluble fibre such as Promitor® and any combination thereof.

In a preferred embodiment of the present invention the bulking agent may be selected from the group consisting of maltodextrins, milk powder (for example skimmed milk powder (SMP)), demineralised whey powder (DWP), soluble wheat or corn dextrin (for example Nutriose®), polydextrose, soluble fibre such as Promitor® and any combinations thereof.

The amorphous porous particles of the invention may comprise (for example consist on a dry basis of) sucrose and skimmed milk, the sucrose being present at a level of at least 30 % in the particles. The ratio of sucrose to skimmed milk may be between 0.5 to 1 and 2.5 to 1 on a dry weight basis, for example between 0.6 to 1 and 1 .5 to 1 on a dry weight basis. The skimmed milk may have a fat content below 1.5 % on a dry weight basis, for example below 1 .2 %. The components of skimmed milk may be provided individually and combined with sucrose, for example the amorphous porous particles of the invention may comprise sucrose, lactose, casein and whey protein. Sucrose and skimmed milk provide an amorphous porous particle which has good stability against recrystallization without necessarily requiring the addition of reducing sugars or polymers. For example, the amorphous porous particles of the invention may be free from reducing sugars (for example fructose, glucose or other saccharides with a dextrose equivalent value. The dextrose equivalent value may for example be measured by the Lane-Eynon method). For further example, the amorphous porous particles of the invention may be free from oligo- or polysaccharides having a three or more saccharide units, for example maltodextrin or starch. The agglomerated amorphous porous particles of the invention may have a moisture content between 0.5 and 6 %, for example between 1 and 5 %, for further example between 1 .5 and 3 %.

In an alternative embodiment of the present invention the amorphous porous particles may comprise no sugar and 100% bulking agent. According to the present invention in a preferred embodiment the amorphous porous particles of the present invention comprise a surfactant or stabilisers which may be necessary to obtain the particles of the present invention with closed pores.

The amorphous porous particles of the invention may comprise for sugar, bulking agent and surfactant, all distributed throughout the continuous phase of the particles. Higher concentrations of the surfactant may be present at the gas interfaces than in the rest of the continuous phase, but the surfactant may be present in the continuous phase inside the particles, not just coated onto the exterior.

In a preferred embodiment, the amorphous porous particles of the present invention comprise a surfactant in the amount of 0.5 to 15%, preferably 1 to 10%, more preferably 1 to 5%, even more preferentially 1 to 3%.

According to the present invention the surfactant may be selected from the group consisting of lecithin, whey proteins, milk proteins, sodium caseinate, lysolecithin, fatty acid salts, lysozyme, sodium stearoyl lactylate, calcium stearoyl lactylate, lauroyl arginate, sucrose monooleate, sucrose monostearate, sucrose monopalmitate, sucrose monolaurate, sucrose distearate, sorbitan monooleate, sorbitan monostearate, sorbitan monopalmitate, sorbitan monolaurate, sorbitan tristearate, PGPR, PGE and any combinations thereof.

In a preferred embodiment of the present invention the surfactant may be sodium caseinate or lecithin.

It will be well understood in the art that in embodiments according to the present invention wherein the bulking agent is derived from milk powder such as skimmed milk powder or demineralised whey powder, sodium caseinate for example is inherently present.

The amorphous porous particles of the invention may be coated, for example they may be coated in a thin layer of fat such as cocoa butter. A thin layer of fat further enhances the stability of the particles during transport and storage. The porous nature of the amorphous particles of the invention may lead to them being lighter in colour than solid crystalline materials such as sucrose crystals. This can be counteracted by the addition of opaque or coloured materials. The amorphous porous particles of the invention may comprise coloured ingredients, for example caramelized sugars or permitted food colours, for example natural food colours. According to the present invention there is provided a process for preparing the amorphous porous particles of the present invention.

In a preferred embodiment, the amorphous porous particles of the present invention are prepared according to conventional spray-drying methods as here below described.

In a preferred aspect of the present invention there is provided a process to prepare the amorphous porous particle of the present invention comprising in its broad aspects the steps of: subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar;

adding gas to the mixture;

spraying and drying the mixture to form amorphous porous particles; and

reducing the particle size of the amorphous porous particles.

The gas may be added before the mixture has been pressurised. In that case the gas may be added at low pressure into the mixture and then pressurised at a later stage in the process line before spray-drying, for example it may be pressurised such that it dissolves in the mixture. However, the process of compressing a gas/liquid mixture can be difficult to control, so preferably the mixture is pressurised before gas is added, in other words gas may be added to the pressurised mixture.

Accordingly in preferred embodiment of the invention there is provided a process of making the amorphous porous particles comprising the steps of;

subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, for example a pressure of 50 to 300 bars;

adding gas to the said mixture;

spraying and drying the said mixture to form agglomerated amorphous particles; and deagglomerating the said particles to obtain amorphous porous particles having a reduced particle size.

In one preferred embodiment there is provided a process of the present invention wherein the Deagglomeration is carried out by subjecting the agglomerated amorphous particles to high shear mixing.

In one preferred embodiment, there is provided a process of the present invention wherein deagglomeration is carried out by any type of mechanical milling such as cone milling or air-classifier milling or jet-milling or more preferably hammer milling.

The deagglomeration is preferably carried out by hammer milling. The Mesh sizes used for said hammer milling are preferably between 0.1 and 0.4 mm, more preferably between 0.15 and 0.35 mm, even more preferably between 0.2 and 0.35 mm.

In a further embodiment, the hammer milling is carried out preferably at speeds of between 1000 and 8000 rpm, preferably 1500 and 7500 rpm and even more preferably 2000 and 7000 rpm. The hammer mill may be in either hammer or knife configurations.

In a further embodiment there is provided a process of the present invention wherein the deagglomeration of the amorphous porous particles may be carried out in fat based matrix for example vegetable oil or cocoa butter or liquefied chocolate or chocolate

Preferably the agglomerated amorphous porous particles of the invention is mixed with fat, for example any oil such as vegetable oil, cocoa butter or liquefied chocolate or chocolate.

The deagglomeration is preferably carried out by high shear mixing using high shear mixers know in the art such as high shear stator-rotor mixers. The high shear mixing is carried out at high speeds between preferably between 1000 and 6000 rpm, more preferably between 2000 and 4000 rpm In a preferred embodiment of the present invention, the mixture comprising sugar, bulking agent and surfactant may be mixed with 30% water, preferably 40% water and more preferably 50% water until full dissolution is achieved. In a preferred embodiment of the present invention the mixture comprising sugar, bulking agent and surfactant is subjected to high-pressure typically 50 to 300 bar, preferably 100 to 200 bar, more preferably 100 to 150 bar.

The gas is preferably dissolved in the mixture before spraying, the mixture comprising dissolved gas being held under high pressure up to the point of spraying. Typically the gas is selected from the group consisting of nitrogen, carbon dioxide, nitrous oxide, air and argon. Preferably the gas is nitrogen and it is added for as long as it takes to achieve full dissolution of gas in the said mixture. For example the time to reach full dissolution may be at least 2 minutes, for example at least 4 minutes, for further example at least 10 minutes, for further example at least 20 minutes, for further example at least 30 minutes. The drying may be spray-drying, for example the spraying and drying may be spray-drying. The pressurised mixture may be sprayed dried according to well-known prior art conventional spray-drying techniques. A skilled person in the art would recognise all the obvious embodiments of using the conventional spray-drying methods well known in the art.

In an alternative embodiment it is plausible that other known procedures may be used to carry out the process of the present invention for example, foam drying, freeze drying, tray drying, fluid bed drying and the like.

According to the present invention the Spray-drying parameters are adjusted to create agglomerated particles as these are easier to store, transport and handle in factories without issues such as dust generation or caking. However, large agglomerates may lead to undesirable mouthfeel attributes such as powdery-ness and grittiness and so, in a product such as a fat based confectionery product it is generally desirable to reduce the particle size of the solid ingredients. It is advantageous that the porosity of the amorphous particles of the invention is able to survive size reduction processes used in chocolate manufacture such as high shear mixing. Pores of approximately spherical shape provide a strong structure to the particles and having multiple small closed pores means that the particles can be fractured without significant loss of internal porosity.

In a further aspect the present invention also provides for amorphous porous particles obtained by the said method as described herein.

According to a general aspect of the present invention, the amorphous porous particles of the present invention have a wide range of utilities, including all of the applications in dry food mixes for which sugar is normally employed. For instance, said particles of the present invention may be used in a variety of food products for example, a confectionery product, a culinary product, a dairy product, a nutritional formula, a breakfast cereal or an ice-cream. In one preferred aspect of the present invention the focus is on the use of the amorphous porous particles to replace sugar in confectionery products (including both fat and sugar based confectionery products). In an embodiment, the invention provides a food product wherein amorphous porous particles have been deagglomerated. In the context of the present invention, the term deagglomerated further refers to material which has been subjected to a process to reduce the particle size of the material's solids.

In the present invention the term 'confectionery product' or 'fat-based confectionery product' is to be understood as meaning chocolate product, chocolate-like product (e.g., comprising cocoa butter replacers, cocoa butter equivalents or substitutes), a coating chocolate, a chocolate-like coating product, a coating chocolate for ice-creams, a chocolate-like coating for ice-cream, a praline, a chocolate filling, a fudge, a chocolate cream, an extruded chocolate product or the like. The fat-based confectionery product may be a white chocolate; comprising sugar, milk powder and cocoa butter but not dark cocoa material. The product may be in the form of an aerated product, a bar, or a filling, among others. The chocolate products or compositions can be used as coatings, fillers, enrobing compositions or other ingredients in a finished or final food or confectionery product. The confectionery product of the invention may further contain inclusions such as nuts, cereals, and the like.

In an alternative embodiment, confectionery product also includes non-fat based confectionery products such as conventional sugar confectionery. According to the knowledge of the skilled person the confectionery products comprising the amorphous porous particles of the present invention may also be used as a filling between biscuits (for example wafers), as part of a coating or as a coating. It can also comprise inclusions such as nuts, puffed cereal, chocolate chips, sugar chips, fruit pieces, caramel pieces, biscuits, wafers, creams or the like. In a preferred embodiment of the present invention there is provided a fat based confectionery composition comprising c) cocoa powder or cocoa liquor or cocoa butter or cocoa butter equivalents or any combinations thereof and d) 5 to 60 wt% of amorphous porous particles according to the present invention wherein said amorphous porous particles comprise sugar, a bulking agent and a surfactant, and wherein said amorphous porous particles have a closed porosity of at least 40% or between 20 to 60%.

In a preferred embodiment of the present invention there is provided a fat based confectionery composition comprising a) cocoa powder or cocoa liquor or cocoa butter or cocoa butter equivalents or any combinations thereof and b) 5 to 60 wt% of amorphous porous particles according to the present invention wherein said amorphous porous particles comprise sugar, a bulking agent and a surfactant, and wherein said amorphous porous particles have a closed porosity of at least 40% and wherein between 10 to 40% of said particles are non-spherical particles.

In a further preferred embodiment there is provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention, comprising the steps of

subjecting a mixture comprising sugar, bulking agent and surfactant to high pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar; adding gas to the mixture; spraying and drying the mixture to form agglomerated amorphous porous particles; mixing ingredients selected from the group consisting of milk powder, fat, cocoa liquor, crystalline sugar, lecithin and any combinations of these; refining the resulting mixture; liquefying the resulting refined mixture with further fat, and optionally lecithin reducing the particle size of the amorphous porous particles; and then adding the particle-size-reduced amorphous porous particles to the refined mixture before or after liquefying. In a further preferred embodiment there is provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention, comprising the steps of

a) subjecting a mixture comprising sugar, bulking agent and surfactant to high

pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar;

b) adding gas to the mixture;

c) spraying and drying the mixture to form agglomerated amorphous porous particles; d) reducing the particles size of the amorphous porous particles

e) mixing ingredients selected from the group consisting of milk powder, cocoa butter, cocoa liquor, crystalline sugar, lecithin and any combinations of these;

f) refining the resulting mixture

g) liquefying the resulting refined mixture with further fat and optionally lecithin and the said amorphous porous particles and liquefying.

In a preferred embodiment there is a provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention wherein the said amorphous porous particles are reduced in size (for example deagglomerated) by high shear mixing or deagglomerated by hammer-milling.

In a further embodiment there is provided a process of the present invention wherein the deagglomeration of the amorphous porous particles may be carried out in fat based matrix for example vegetable oil or cocoa butter or liquefied chocolate or chocolate mass

Preferably, the agglomerated amorphous porous particles of the invention are preferably mixed with fat, for example, any oil such as vegetable oil, cocoa butter or liquefied chocolate to chocolate mass

The liquefaction may for example be performed by conching. The fat may for example be cocoa butter, cocoa butter equivalent or cocoa butter replacer.

In a further embodiment there is a provided a process of making a fat based confectionery product comprising the amorphous porous particles of the present invention wherein the said amorphous porous particles are reduced in particle size by high shear mixing

The deagglomeration of the powder directly, for example the amorphous porous particles of the present invention may also be subjected to direct high shear mixing.

In another embodiment the reduced particle size amorphous porous particles may be added after the refining step and before the liquefaction step.

The gas may be added before the mixture has been pressurised. In that case the gas is pressurised together with the mixture, for example it may be pressurised such that it dissolves in the mixture. Preferably, the mixture is pressurised before gas is added.

The fat may for example be cocoa butter, cocoa butter equivalent or cocoa butter replacer. The fat may be cocoa butter. Some or all of the milk powder, cocoa liquor and crystalline sugar may be replaced by chocolate crumb. In a preferred embodiment, the liquefaction is carried out by conventional means well known to a person skilled in the art and refers to conching, a standard process in chocolate manufacture. The reduction of particle size may be such that the resulting amorphous porous particles have a D90 particle size distribution of between Of between 100 and 200 microns, more preferably 1 10 and 170 microns and even more preferably 1 10 and 160 microns

Roll refiners may be used to refine the mixture, for example, a combination of 2-roll and 5- roll refiners may be used to refine the mixture.

Agglomerated powders provide advantages as ingredients in terms of flowability and lower dustiness. For example, the amorphous porous particles may be amorphous porous particles according to the invention agglomerated as part of a spray-drying process, for example an open top spray drier with secondary air recirculation to trigger particle agglomeration. The agglomerated particles may have a particle size distribution D90 of between 120 and 600 microns preferably 120 and 450 microns. The invention may provide a fat based confectionery composition comprising

a) cocoa powder or cocoa liquor or cocoa butter or cocoa butter equivalents or any combinations thereof and b) 5 to 60 % of amorphous porous particles according to the present invention. wherein said amorphous porous particles comprise (for example consist on a dry basis of) sucrose and skimmed milk, the sucrose being present at a level of at least 30 % in the particles, the ratio of sucrose to skimmed milk being between 0.5 to 1 and 2.5 to 1 on a dry weight basis, for example between 0.6 to 1 and 1 .5 to 1 on a dry weight basis. It is advantageous that the fat based confectionery composition may comprise only ingredients commonly found in fat based confectionery products such as chocolate. The amorphous porous particles comprised within the fat based confectionery may be free from reducing sugars and/or free from oligo- or polysaccharides having a three or more saccharide units. In a preferred embodiment to the present invention, the fat based confectionery product comprises 5 to 60% of the amorphous porous particles, preferably 10 to 50%, more preferably 20 to 40%.

All terms such as amorphous, porous, sugar, surfactant and bulking agent are as previously defined.

In a preferred embodiment the fat based confectionery product comprises amorphous porous particles having a glass transition temperature of at least 40°C or higher. In another preferred embodiment, the fat based confectionery product comprises amorphous porous particles having a D90 particle size of between 100 and 200 microns, more preferably 1 10 and 170 microns and even more preferably 1 10 and 160 microns

According to the present invention, the fat based confectionery product comprising the amorphous porous particles of the present invention is prepared according to conventional chocolate making processes as will be well known and obvious to a person skilled in the art.

In a further embodiment of the present invention there is provided a process of making a fat based confectionery product comprising amorphous porous particles comprising the steps of: subjecting a mixture (for example an aqueous mixture) comprising sugar, bulking agent and surfactant to high pressure, preferably 50 to 300 bar, more preferably 100 to 200 bar;

adding gas to the mixture;

spraying and drying the mixture to form agglomerated amorphous porous particles; mixing the amorphous porous particles with fat and optionally ingredients selected from the group consisting of milk powder, cocoa liquor, crystalline sugar, lecithin and combinations of these, preferably at a temperature between 35 and 55°C for 2 to 20 minutes;

refining the resulting mixture; and

mixing the refined mixture with further fat and optionally lecithin and liquefying.

The gas may be added before the mixture has been pressurised. In that case, the gas is pressurised together with the mixture, for example it may be pressurised such that it dissolves in the mixture. Preferably, the mixture is pressurised before gas is added. The fat may for example be cocoa butter, cocoa butter equivalent or cocoa butter replacer. The fat may be cocoa butter. Some or all of the milk powder, cocoa liquor and crystalline sugar may be replaced by chocolate crumb. In a preferred embodiment, the liquefaction is carried out by conventional means well known to a person skilled in the art and refers to conching, a standard process in chocolate manufacture. The reduction of particle size may be such that the resulting amorphous porous particles have a D90 particle size distribution of between Of between 100 and 200 microns, more preferably 1 10 and 170 microns and even more preferably 1 10 and 160 microns

Roll refiners may be used to refine the mixture, for example, a combination of 2-roll and 5- roll refiners may be used to refine the mixture. Agglomerated powders provide advantages as ingredients in terms of flowability and lower dustiness. The amorphous porous particles mixed with fat before refining may be in the form of an agglomerated powder. For example, the amorphous porous particles may be amorphous porous particles according to the invention agglomerated as part of a spray- drying process, for example an open top spray drier with secondary air recirculation to trigger particle agglomeration. The agglomerated particles may have a particle size distribution D90 of between 120 and 600 microns preferably 120 and 450 microns.

Advantageously the impact of the high shear mixing and the impact of the hammer milling do not destroy the particles of the present invention. Further, advantageously, the harsh processing conditions of the chocolate making process such as refining does not destroy the porosity of the particles of the present invention, for example, the particle size of agglomerated particles described above could be reduced by high shear mixing whilst still retaining much of their original closed porosity. For example, after high shear mixing the particles may retain at least 20 %, 30 %, 40 % or 50 % of their initial closed porosity, for further example the particles after high shear mixing may have a closed porosity between 20 and 60%. Furthermore, it was surprisingly found that deagglomerated particles of the present invention retained their porosity with no release of the internally contained gas bubbles This was reflected in the food products such as the lighter coloration of for example chocolate products comprising the said particles of the present invention. Particles formed by spray drying are generally spherical in form but when formed into agglomerates, the particles are less spherical.

Imaging experiments show clearly that the particles of the present invention retain significant porosity after deagglomeration by high shear mixing. Sensory evaluations performed showed good tasting qualities and light and creamy texture and mouthfeel indicative of particle porosity remaining intact within the product.

The amorphous porous particles may comprise (for example consist on a dry basis of) sucrose and skimmed milk, the sucrose being present at a level of at least 30 % in the particles, the ratio of sucrose to skimmed milk being between 0.5 to 1 and 2.5 to 1 on a dry weight basis, for example between 0.6 to 1 and 1.5 to 1 on a dry weight basis.

As explained above, agglomerated material possesses improved handling properties such as flowability and lower dustiness. Thus, in a preferred embodiment the agglomerated particles according to the invention may have rounded surfaces composed of the surfaces of individual spherical particles. The agglomerated particles may have at least 70 % of their surface being convex. The agglomerated particles may comprise fewer than 20 (for example fewer than 10) spherical particles. The agglomerated particles may have a particle size distribution D90 of between 120 and 600 microns, preferably 120 and 450 microns

In the following description reference is made to the use of the amorphous porous particles of the present invention as bulk sugar replacers in fat based confectionery products as a preferred embodiment,. The amorphous porous particles of the present invention may however also be used in a wide range of food products as aforementioned.

In the present invention, the term bulk sugar replacer as used herein refers to a low or no calorie sugar substitute that can be substituted at a weight to weight and/or volume to volume basis for sugar. As aforementioned, the combination of the amorphous highly porous sugar particles and bulking agent provide a synergistic effect whereby a further bulking effect is achieved through aeration. In one aspect of the present invention, this advantageously provides up to at least 70% sugar reduction in a food product for example a fat based confectionery product. Preferably, at least 65% of sugar may be reduced from a food product such as a fat based confectionery product. Preferably, between 5 to 70% of sugar may be reduced or removed from a food product such as a fat based confectionery product.

In an embodiment of the invention where the amorphous porous particles are comprised within a fat based confectionery composition and the particles comprise (for example consist on a dry basis of) sucrose and skimmed milk, increasing the proportion of skimmed milk to sucrose reduces the amount of sucrose in the overall fat based confectionery composition. This can be advantageous, as many consumers would welcome a good tasting fat based confectionery with reduced sugar, and appreciate a high milk content. Reducing the proportion of sucrose in the particles reduces their sweetness directly, but it also reduces the dissolution speed of the particles which further reduces sweetness impact in the mouth. However, the inventors have found that by increasing the porosity of the particles, in particular the closed porosity of the particles, they can increase the dissolution speed and so counteract that reduction of sweetness. Accordingly, the invention may provide a fat based confectionery composition comprising

a) cocoa powder or cocoa liquor or cocoa butter or cocoa butter equivalents or any combinations thereof and b) 5 to 60 % (for example 20 to 55 %) of amorphous porous particles according to the present invention. wherein said amorphous porous particles have a moisture content of between 1 % and 5 % (for example between 2 % and 3 %), comprise sucrose and skimmed milk at a level of at least 95 % of the particles on a dry basis (for example at least 98 %), have a ratio of sucrose to skimmed milk between 0.5 : 1 and 0.6 : 1 and have a closed porosity between 20 % and 60 %, for example between 25 % and 50 %, for further example between 25 % and 40 %. The amorphous porous particles may have a D90 particle size distribution of between 30 and 60 microns, for example between 35 and 50 microns. The inventors have investigated the impact on the stability of the amorphous porous particles of altering the ratio of sucrose to skimmed milk powder (see example 5). There is a significant decrease in stability when the ratio of sucrose to skimmed milk powder exceeds 0.6: 1 . Therefore, when seeking to reduce the sucrose content in a food product by replacing crystalline sucrose with amorphous porous particles of the invention containing sucrose and skimmed milk an optimum ratio to use is around 0.66: 1 .

In a preferred embodiment of the present invention, the amorphous porous sugar particles of the present invention may be used as a bulk sugar replacer in a food product. The amorphous porous sugar particles of the present invention may be used to reduce the sugar content of a food product. For example the amorphous porous sugar particles may be used to reduce the sugar content (for example the sucrose content) of a fat-based confectionery product by between 50 and 70 % on a volume basis, or to reduce the sugar content (for example the sucrose content) of a fat-based confectionery product by between 10 and 35 % on a mass basis.

In another embodiment of the present invention the amorphous porous sugar particles are preferably used in a food product such as a confectionery product, a culinary product, a dairy product, a nutritional formula, a breakfast cereal or an ice-cream. In an embodiment of the present invention there is provided a sweetener composition consisting of amorphous porous particles comprising, sugar, a bulking agent and a surfactant, wherein said amorphous porous particles have a closed porosity of between at least 40%

Ranges In the discussion of the invention herein, unless stated to the contrary, the disclosure of alternative values for the upper and lower limit of the permitted range of a parameter coupled with an indicated that one of said values is more preferred than the other, is to be construed as an implied statement that each intermediate value of said parameter, lying between the more preferred and less preferred of said alternatives is itself preferred to said less preferred value and also to each less preferred value and said intermediate value.

For all upper and/or lower boundaries of any parameters given herein, the boundary value is included in the value for each parameter. It will also be understood that all combinations of preferred and/or intermediate minimum and maximum boundary values of the parameters described herein in various embodiments of the invention may also be used to define alternative ranges for each parameter for various other embodiments and/or preferences of the invention whether or not the combination of such values has been specifically disclosed herein.

Percentages

Unless otherwise specified % in the present description correspond to wt% It will be understood that the total sum of any quantities expressed herein as percentages cannot (allowing for rounding errors) exceed 100%. For example the sum of all components of which the composition of the invention (or part(s) thereof) comprises may, when expressed as a weight (or other) percentage of the composition (or the same part(s) thereof), total 100% allowing for rounding errors. However where a list of components is non exhaustive the sum of the percentage for each of such components may be less than 100% to allow a certain percentage for additional amount(s) of any additional component(s) that may not be explicitly described herein.

Substantially

The term "substantially" as used herein may refer to a quantity or entity to imply a large amount or proportion thereof. Where it is relevant in the context in which it is used

"substantially" can be understood to mean quantitatively (in relation to whatever quantity or entity to which it refers in the context of the description) there comprises an proportion of at least 80%, preferably at least 85%, more preferably at least 90%, most preferably at least 95%, especially at least 98%, for example about 100% of the relevant whole. By analogy the term "substantially-free" may similarly denote that quantity or entity to which it refers comprises no more than 20%, preferably no more than 15%, more preferably no more than 10%, most preferably no more than 5%, especially no more than 2%, for example about 0% of the relevant whole.

The term "comprising" as used herein will be understood to mean that the list following is non exhaustive and may or may not include any other additional suitable items, for example one or more further feature(s), component(s), ingredient(s) and/or substituent(s) as appropriate. Thus the words "comprise", "comprising" and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is to say, in the sense of "including, but not limited to". It should be noted that embodiments and features described in the context of one of the aspects of the present invention also apply to the other aspects of the invention.

Experimental Section

Determination of Glass transition temperature

Glass transition temperatures (Tg) were measured by Differential Scanning Calorimetry (TA Instrument Q2000). A double scan procedure was used to erase the enthalpy of relaxation and get a better view on the glass transition. The scanning rate was 5 °C/min. The first scan was stopped approximately 30 °C above Tg. The system was then cooled at 20 °C/min. The glass transition was detected during the second scan and defined as the onset of the step change of the heat capacity.

Determination of structures using cryo-scanning electron microscopy Cryo-Scanning Electron Microscopy (Cryo-SEM) and X-ray Tomography (μΰΤ) are used to investigate the microstructure of the amorphous porous particles of the present invention within a fat based food matrix.

A 1 cm 3 piece of sample was glued into a Cryo-SEM sample holder using TissueTek. It was rapidly frozen in slushy nitrogen prior to its transfer into the cryo-preparation unit Gatan Alto 2500 at -170 °C. The frozen sample was fractured using a cooled knife, making its internal structure accessible. The fracture was not performed when the external surface of the chocolate was analyzed. A slight etching of superficial water was performed in the preparation unit for 15 min at -95 °C, followed by sample stabilization at -120 °C. A final coating was done by an application of a 5 nm platinum layer onto the surface. For visualization a FEI Quanta 200 FEG at 8 kV in high vacuum mode was used.

Particle size

The particle size values given herein may be measured by a Coulter LS230 Particle Size Analyser (laser diffraction) or any other similar machine as known to those skilled in the art. In present invention the term particle size as used herein is defined as D90. The D90 value is a common method of describing a particle size distribution. The D90 is the diameter where 90 % of the mass of the particles in the sample have a diameter below that value. The D90 value may be measured for example by a laser light scattering particle size analyser.

The invention will now be described in further details in the following non-limiting examples. The following Examples are provided of illustrative purposes only and they are not to be considered in any way limiting to the scope of the present invention. It should be understood that various changes and modifications to the presently preferred embodiments described herein will be apparent to those skilled in the art. Such changes and modifications can be made without departing from the spirit and scope of the present invention and without diminishing its attendant advantages. It is therefore intended that such changes and modifications be covered by the appended claims. It will be appreciated that if (for example in the Examples herein) the weight percentages herein do not add up to 100% (e.g. due to rounding) they can also be considered as recipes where the same numbers for the weight percentage of each ingredient is considered as a relative part by weight.

Examples The following examples are illustrative of the products and methods of making the same falling within the scope of the present invention. They are not to be considered in any way limitative of the invention. Changes and modifications can be made with respect to the invention. That is the skilled person will recognise many possible variations in these examples covering a wide range of compositions, ingredients, processing methods and mixtures and can adjust the naturally occurring levels of the compounds of the invention for a variety of applications.

Example 1 Preparation of the agglomerated amorphous porous particles of the present invention

Sucrose (60%) and skimmed milk powder (40%) are mixed in water (50%) for about 15 minutes at 60°C, then for a further 5 minutes at 75°C. The homogenous solution is injected into the tube at between 60°C and 70°C, nitrogen is then added before pressurising at 50 to 300 bars. When the solution reaches the nozzle it is spray-dried, in the tower. In this example an open-top industrial spray-drier was used

In an another method all ingredients were weighed separately and then mixed with a polytron PT3000D mixer until full dissolution at room temperature with a speed rate between 6000 and 12000 rpm. The inlet solution is transferred in a vessel at controlled temperature of 55°C and is then pumped at 100-130 bar. High pressure nitrogen is injected at 0.5-3 NL/min to allow full dissolution of the gas in the solution. After a pre-heating at 60°C, the solution is spray-dried using an open-top industrial spray drier according to the parameters listed in the table below:

Solution flowrate 2000-4000L/h

Agglomerated amorphous porous particles of the present invention were prepared in accordance with example 1 , samples were prepared with the following characteristics:

Example 2 Preparation of the deagglomerated amorphous porous particles of the present invention.

The agglomerated amorphous porous particles in amount of 33% were mixed with 66% sunflower oil using a Hobart planetary mixer at speed 2 for 2 minutes, at room temperature to obtain a homogeneous texture. The composition was 1 part by weight powder plus 2 parts by weight sunflower oil. The mixture was filled into a stainless steel cylindrical vessel sealed at the lower end.

The head of a Silverson high shear stator-rotor mixer was fitted with a Square Hole High Shear Screen™ and the mixer head was lowered into the cylinder until just immersed in the mixture. The mixer was started and set at a rotational speed of 3500rpm. The cylinder was then raised at a rate of 10mm/second causing the mixing head to travel through the column of mixture. At the end of travel the mixing head speed was reduced to an idle and the cylinder lowered back down. The mixer was stopped. A sample of the mixture was sampled for analysis and the procedure then repeated up to 3 cumulative passes through the mixing head at the same settings. Samples were taken after each pass.

At the end of treatment the temperature had risen to approximately 50°C due to the mechanical work applied. Changes in rheology were adjudged visually on pouring the slurry. It was observed that the application of the high shear mixing reduced the viscosity of the mixture, indicating deagglomeration and/or particle size reduction of the agglomerated amorphous porous particles of the present invention. The samples had better texture and flowability

Surprisingly, it was found that the even after subjecting the amorphous porous particles of the present invention to high shear mixing conditions a significant proportion of the closed porosity remained intact and/or at acceptable levels, the said particles of the invention having closed porosity levels ranging from between 45% to over 50% or between 20 and 60%.

Example 3

Preparation of non-agglomerated or primary particles of the present invention

All ingredients were weighed separately and then mixed with a polytron PT3000D mixer until full dissolution at room temperature with a speed rate between 6000 and 12000 rpm. The inlet solution is transferred in a vessel at controlled temperature of 55°C and is then pumped at 100-130 bar. High pressure nitrogen is injected at 0.5-2 NL/min for at least 10 mins or a least until full dissolution of the gas in the solution is achieved. After a pre-heating at 60 0 C, the solution is spray-dried using a one stream closed-top spray drier according to the parameters listed in the table below:

Gas injection 0.5-2 NL/min

Solution flowrate 12 L/h

Non-agglomerated Amorphous porous particles (herein referred to as the primary particles or non-agglomerated powder or Powder 3) were prepared as in Example 3, with the inlet solution containing 50 wt% water and 50 wt% of (sucrose + SMP (skimmed milk powder) in ratio of 60:40). No sodium caseinate was added as this is already present in SMP.

Advantageously, the deagglomerated amorphous porous particles powders of the present inventions have comparable closed porosity to the non-agglomerated primary particles as prepared by conventional spray-drying methods according to example 3. Powder 1 has a closed porosity of 55.8%, Powder 2 has a closed porosity of 50.8 % and both values are similar to the non-agglomerated amorphous porous particles which have a closed porosity of 53 %.

Example 4

Preparation of the deagglomerated amorphous porous particles of the present invention. The agglomerated porous particles as prepared according to Example 1 were subjected to hammer milling using the HammerWitt-Lab or HammerWitt-3 milling device from Frewitt.

The amorphous porous particles prepared according to Example 1 were fed into the mill grinding chamber through the feed chute by gravity. The particles were repeatedly struck by ganged hammers which are attached to a shaft rotating at high speed inside the mill chamber. The material was crushed or shattered by a combination of repeated hammer impacts, collisions with the walls of the grinding chamber, and particle on particle impacts. Perforated metal screen covering the discharge opening of the mill retained coarse material for further grinding, while allowing properly sized materials to pass as finished product. Three different mesh sizes of 0.200 mm, 0.250mm and 0.315mm and speeds between 2000 rpm and 7000 rpm were used.

The effect of altering the mesh sizes and rotation speeds on the porosity and particle size distribution was investigated. Amorphous porous particles were prepared as in Example 1 , with the inlet solution containing 50 wt% water and 50 wt% of sucrose (60 wt%) + SMP (40 wt%) (skimmed milk powder). No sodium caseinate was added as this is already present in SMP. This was then subsequently deagglomerated using hammer milling according to Example 4.

Powder 2 was deagglomerated using hammer milling according to Example 4 and samples with the same composition but with different combinations of mesh sizes and speeds were prepared

Powder 1 was deagglomerated using hammer milling according to Example 4 and samples with the same composition and with the same mesh size of 0.250 mm but with different speeds were prepared

8 3000 51.7 132.9 78 40.3

9 4000 51.5 132.1 76.9 39.8

10 5000 50.6 128.7 72.1 36.2

1 1 6000 48.6 120.9 70.8 35.6

12 7000 46.5 1 12.4 66.9 31.7

Surprisingly, it was found that the even after subjecting the amorphous porous particles of the present invention to harsh milling conditions a significant proportion of the closed porosity remained intact and/or at acceptable levels, the said particles of the invention having closed porosity levels ranging from between 45% to over 50%. Example 5a

Assessment of the morphology of the amorphous porous particles of the present invention by a visual texture test

Samples prepared according to Example 4, were mixed with cocoa butter (55% of the deagglomerated powder mixed in with 45% cocoa butter) in order to assess the flowability and viscosity of the particles of the present invention in a fat based matrix. Surprisingly it was found that, at a visual scale there was no difference in flowability and viscosity compared to the non-agglomerated amorphous particles prepared according to Example 3.

The samples were prepared by dipping the mixtures on to microscope slides to test visually viscosity and texture or flowability. It is desirable to obtain a fluid texture with cocoa butter a key chocolate manufacturing ingredient. Advantageously the cocoa butter mixtures comprising the deagglomerated amorphous porous particles of the present invention provided good consistency, generating good fluid texture with derisible viscosity and flowability. The results indicate that samples with particle size distributions above D90 100 microns, for example, mix well with cocoa butter yielding fluid texture. Example 5b

Powder shape morphology

Assessment of the impact of shape of the amorphous porous particles of the present invention on the fluid texture with cocoa butter was also assessed. Powder shape plays an important role on viscosity due to the importance of the exchange area to be coated by cocoa butter and the free space to move enabling easy flow. As a rule, the more spherical the more easily the particles flow thanks to a better packing.

To enable the morphology characterization, the following parameter of sphericity was used and further defined as:

4πΑ

P 2

With A is defined as the measured area covered by a particle projection and P is the measured perimeter of a particle projection The limit of 0.90 was defined as the limit of round particles. Above 0.90, particles are considered as round and below 0.90, they are considered as not round. Samples prepared according to the methods of the present inventions were assessed for the percentage of non-spherical particles using the Morphological device (Malvern, UK).

The table of shows that non-agglomerated particles (Powder 3) contain less non spherical particles around 10.61 % and the agglomerated amorphous porous particles made according to the present invention contain 51 .39 % non-spherical particles. Samples 7 to 8 deagglomerated by hammer milling according to Example 4, have between 19 and 25 % non-spherical particles. Advantageously Hammer milling significantly reduces the percentage of non-spherical particles.

Optimum values for acceptable morphology for the deagglomerated amorphous porous particles of the present invention are a particle size D90 of 150 microns and a maximum of 20% of non-spherical particles.

It is well known in the art that porosity is linked to dissolution and sweetness perception which is maintain even at lower levels of closed porosity for example of at least 40% closed porosity Example 6

A standard reference formulation for a chocolate recipe

A standard process for the preparation of chocolate was employed. All dry ingredients and about 26% of cocoa butter fat is heated at 45 °C for 3 mins. After mixing, the resulting paste is passed through a two roller refiner and a five roller refiner to produce flakes with particle sizes ranging between 50 and 55 microns.

After refining, the mixture comprising the refined mass is mixed with the rest of the fat and lecithin to liquefy it at 45 °C for 3 mins.

A reduced sugar chocolate composition was prepared according to the standard recipe using SMP 60:40 in the form of deagglomerated amorphous porous powder.

Surprisingly it was found that by replacing the sugar with 100% of the amorphous porous particles of the present invention in chocolate recipes as described in the example above provided chocolate samples closely matched the reference sample in terms of texture, flavour and sweetness. Similar results were also obtained for fat based confectionery filling recipes, for example wafer filling recipes.

In addition the samples prepared according to the present invention and comprising the amorphous porous particles instead of sugar showed a strong correlation with additionally desirable flavours such as milky, caramel, vanilla and butter.

Example 6 The effect of altering the composition of the amorphous matrix was examined for different ratios of skimmed milk powder (SMP) and sucrose. The amorphous matrix should be stable against crystallization, for example, in the case of chocolate manufacture the matrix should remain amorphous under the temperature and humidity conditions experienced in the conche. If processing or storage conditions approach those at which the amorphous material passes through the glass transition then there is a possibility that crystallization will occur leading to a collapse of the particles, for example the lactose present in amorphous porous particles of skimmed milk powder and sucrose may crystallize.

Amorphous porous particles with different ratios of sucrose:SMP were produced; 40:60, 50:50, 60:40, 70:30 and compared to pure amorphous sucrose and SMP. The amorphous SMP was spray dried. The amorphous sucrose was obtained by freeze drying (Millrock, US). A solution containing10% (weight basis) of sucrose was prepared. It was frozen at - 40 °C for 6 hours allowing the formation of ice crystals. Primary drying is performed at 150 mTorr. Ice crystals sublimate and leave voids behind leading to a highly porous structure. Secondary drying consists of a temperature ramp from -40 °C to 40 °C at 1 °C/hour. During that stage residual water bound to the matrix is removed by desorption leading very low moisture content, typically 1 -2% as measured by ThermoGravimetric Analysis.

As the samples initially have different water activity (Aw) values the sorption isotherms were drawn to calculated Tg at the same a w . 1) Sorption isotherms were built by collecting samples during short periods of time (i.e. typically over 48h) stored in two types of desiccators (one for partial drying and one for humidification). The Tg of each sample was obtained by using the second scan of DSC experiment at 5 °C/min heating ramp. The first scan should stop at about 30 °C above the T g in order to avoid relaxation enthalpy interference with T g measurement. Onset T g of the product is then determined using a second scan. After 2h heating at T g +5°C <¾ is measured at 25°C.

2) BET fitting is performed over the data of moisture content as a function of aw (0.08- 0.35) and the Gordon Taylor over the data of Tg as a function of a w (corresponding range). a. Brunauer-Emmett-Teller equation (BET):

M fa M ^ C a w

d b ( w ) " (l - a w ) [l + (C - l) aj where Cis a constant and M m is the BET monolayer moisture content (on dry basis)

b. Gordon-Taylor equation (Gordon and Taylor, 1952):

j, _ fcw ¾,w ter+(l ~w ) 7 'g,dry

9 ~ fcw + fc(l-w) where w is water content on a weight basis, T g , W ater is the glass-transition temperature of water estimated at -135 °C, T g ,d ry is the glass-transition temperature of sucrose and k is a curvature constant.

The glass transition temperature (Tg) is plotted against sucrose content in Figure 3 for amorphous particles at a water activity of 0.1 and 25 °C. It can be seen that there is a much more pronounced decrease in glass transition temperature for increasing sucrose content at or above 40 % (a ratio of 0.66 : 1 ). This means that there is a significant decrease in stability (against crystallization) when the level of sucrose in an amorphous matrix containing sucrose and skimmed milk powder exceeds 40 %. Therefore, when seeking to reduce the sucrose content in a food product by replacing crystalline sucrose with amorphous porous particles of the invention containing sucrose and skimmed milk an optimum proportion to use is around 40 % sucrose and 60 % skimmed milk powder.

Example 7

A white chocolate was prepared using agglomerated amorphous porous particles which were prepared according to Example 1 and then subsequently deagglomerated according to Example 2. For the preparation of the agglomerated amorphous porous particles; sucrose (40%) and skimmed milk powder (60%) were mixed with water at a total solids of 50% until all solids dissolved at a temperature of around 60 °C. After pasteurization (5 minutes at 75 °C), the homogeneous solution was spray dried with gas injection. The spray drier used was an open top spray drier with secondary air recirculation to trigger particle agglomeration. The solution temperature was controlled between 60 and 70 °C and nitrogen was added under pressure in a similar manner to Example 1 . The output powder moisture content was 20 - 30 g/kg The powder had a closed porosity of 55.8% and a particle size distribution D90 of 160 μπι.

The powder was then deagglomerated using high shear mixing according to example 2 to obtain deagglomerated amorphous porous particles with a D90 particles size of 130.1 microns and closed porosity of 46.9%

White chocolate was manufactured using this de-agglomerated amorphous porous powder:

The following dry ingredients milk powder , cocoa butter, crystalline sugar and lecithin were mixed at around 50 °C for 15 minutes. After mixing, the resulting paste was passed through a two-roll refiner and a five-roll refiner to produce flakes.

After refining, the resulting refined mixture was liquefied by conching using a Frisse-conche with further fat, and optionally lecithin. Then the agglomerated amorphous porous particles were deagglomerated using a Silverson high-shear mixer and subsequently added to liquefied chocolate. The chocolate was tempered and moulded into tablets. A reference tablet was made in the same manner as above, but the amorphous porous powder was replaced at 1.9 times its mass by crystalline sucrose; effectively occupying the same volume as the replaced amorphous porous powder.

A small panel of tasters compared the chocolate made with amorphous porous powder to the reference chocolate. The same sized piece was taken of each. Due to the different densities of the powders the tasted pieces contained different amounts of sugar by weight. The chocolate made with amorphous porous powder was described as slightly more "powdery" but with a similar sweetness to the reference. This is despite it containing 68 % less sucrose for the same volume.

Example 8 A white chocolate was prepared using agglomerated amorphous porous particles which were prepared according to Example 1 and then subsequently deagglomerated according to Example 4.

For the preparation of the agglomerated amorphous porous particles; sucrose (40%) and skimmed milk powder (60%) were mixed with water at a total solids of 50% until all solids dissolved at a temperature of around 60 °C. After pasteurization (5 minutes at 75 °C), the homogeneous solution was spray dried with gas injection. The spray drier used was an open top spray drier with secondary air recirculation to trigger particle agglomeration. The solution temperature was controlled between 60 and 70 °C and nitrogen was added under pressure in a similar manner to Example 1 . The output powder moisture content was 20 - 30 g/kg The powder had a closed porosity of 55.8% and a particle size distribution D90 of 160 μπι.

The powder was then milled using a hammer mill according to example 2 using a mesh size 0.315 mm and speed of 5000 rpm to obtain deagglomerated amorphous porous particles with a D90 particles size of 130.1 microns and closed porosity of 46.9% White chocolate was manufactured using this de-agglomerated amorphous porous powder:

Ingredients Amount (wt%)

Cocoa butter 23

Milk powder (whole and skimmed) 54

Milk fat 4

Crystalline sucrose 4.5

Amorphous porous powder 14 Lecithin and vanilla 0.5

The following dry ingredients milk powder, cocoa butter, crystalline sugar and lecithin were mixed at around 50 °C for 15 minutes. After mixing, the resulting paste was passed through a two-roll refiner and a five-roll refiner to produce flakes. After refining, the refined mass and the deagglomerated amorphous porous particles were conched in a Frisse conche with the addition of the remaining cocoa butter, the milk fat, lecithin and vanilla. The chocolate was tempered and moulded into tablets.

A reference tablet was made in the same manner as above, but the amorphous porous powder was replaced at 1 .9 times its mass by crystalline sucrose; effectively occupying the same volume as the replaced amorphous porous powder.

A small panel of tasters compared the chocolate made with amorphous porous powder to the reference chocolate. The same sized piece was taken of each. Due to the different densities of the powders, the tasted pieces contained different amounts of sugar by weight. The chocolate made with amorphous porous powder was described as slightly more "powdery" but with a similar sweetness to the reference. This is despite it containing 68 % less sucrose for the same volume.




 
Previous Patent: WALL ELEMENT

Next Patent: SYNTENIN INHIBITORS AND USES THEREOF