WO2000033673A1

WO2000033673A1 - Microparticles and process for making microparticles

Info

Publication number: WO2000033673A1
Application number: PCT/IB1999/001939
Authority: WO
Inventors: Patricia-Ann Truter; Patience Makhosaxana Xulu; Nicholas Afamefuna Igwe
Original assignee: Csir
Priority date: 1998-12-08
Filing date: 1999-12-06
Publication date: 2000-06-15
Also published as: AU1291800A

Abstract

An edible capsule is provided having a predetermined density and which is configured to be suspended in a liquid, the capsule includes at least one edible functional ingredient and an edible water insoluble particle-forming encapsulating agent which encapsulates the functional ingredient and which inhibits diffusion of the functional ingredient from the capsule. The invention extends to a process for preparing edible capsules, and to a beverage which includes edible capsules.

Description

MICBOPARTICLES AND PROCESS FOR MAKING MICROPARTICLES

THIS INVENTION relates to capsules. It also relates to a process for making capsules and to a beverage.

According to a first aspect of the invention, there is provided an edible capsule having a predetermined density and which is configured to be suspended in a liquid, the capsule including at least one edible functional ingredient; and an edible water insoluble particle-forming encapsulating agent which encapsulates the functional ingredient and which inhibits diffusion of the functional ingredient from the capsule.

Thus, the diffusivity of the functional ingredient through the encapsulating agent may be less than 0,001 cm Is, preferably less than 0,0005 cm²/s, and most preferably less than 0, 1 X 10^~5cm²/s.

The functional ingredient may be a food grade pigment or a preservative or a dye. Instead, the functional ingredient may be a biologically active ingredient.

The biologically active ingredient may be selected from the group consisting of energy source materials, amino acids, vitamins, creative homeopathic remedies, electrolytes, minerals, trace minerals, medicaments, enzymes, herbalextracts, muscle-builders, appetitesuppressants, performance enhancement substances, and mixtures thereof. Examples of suitable vitamins are vitamin A (Retinol), vitamin B- complex, vitamin B1 (thiamine) , vitamin B2 (riboflavin), vitamin B3 (niacin/niacinamide) , vitamin B5 (pantothenic acid), vitamin B6 (pyridoxine), vitamin B8 (folic acid), vitamin B1 2 (cobalamin) , vitamin C (ascorbic acid), vitamin D (colecalciferol), vitamin E (tocopherol), vitamin K (phylloquinone), and mixtures of these.

Examples of suitable amino acids are alanine, arginine, asparagines, aspartic acid, cystine, glutamine acid, glycine, histidine, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tryptophan, tyrosine, valine, carnitine, branched chain amino acids, or the like.

Examples of suitable herbal extracts are Siberian ginseng,

Manchurian ginseng, grape seed extract, green tea extract, Hawthorn extract, garlic, ginger, Gingko Biloba extracts, calendular extract, aloe vera, chamomile, Hawthorn berries, comfrey, alfa alfa, kelp, spirulina, Tribulis

Terestris extract, muira puama extract, or the like.

Examples of other substances which may be encapsulated as a functional ingredient are bioflavonoids, citrus bioflavonoids, L-carnitine, hydroxy citrate, co-enzyme Q1 0, creatin monohydrate, medium chain triglycerides, lecithin, royal jelly, brewer's yeast, soy protein, whey protein and beta hydroxy-beta-methylbutyrate.

When the active ingredient is an energy source material, it may be selected from the group consisting of sugars, starches, simple carbohydrates, xylitols, artificial sweeteners, and mixtures thereof. Examples of specific energy source materials are glucose, sucrose, fructose, dextrose monohydrate, saccharin, sodium cyclamates, sucralose, aspartame and lactitol. When the active ingredient is a mineral, it may be selected from the group consisting of iron, magnesium, fluoride, calcium, phosphorus, manganese, iodine, copper, zinc, potassium, selenium, chromium, and mixtures thereof.

When the active ingredient is a trace mineral, it may be selected from the group consisting of selenium, zinc, and mixtures thereof.

The capsule may contain between 0.01 % by mass and 10% by mass of the functional ingredient. Typically, the capsule contains between 2% by mass and 5% by mass of the functional ingredient.

The water insoluble particle-forming encapsulating agent may be a material or polymer which is biodegradable or biocompatible.

The functional ingredient may be oxidizable. Thus, the capsule may include an antioxidant or an oxygen scavenger to inhibit oxidation of the functional ingredient, e.g. butylated hydroxy toluene or ethoxyquin.

The capsule may include at least one density modifying agent which modifies the density of the capsule to a predetermined extend thereby permitting the capsule to be suspended in a preselected liquid of particular density.

The capsule may be in the form of a bead or microsphere, or the like, having a polymeric coating or shell or encapsulating agent which encapsulates a core containing the functional ingredient and the density modifying agent.

The density modifying agent may be a liquid, e.g. an oil. The oil may have a density less than that of water at the same temperature. Thus, the function of the density modifying agent may be to reduce the density of the capsule. The oil may be selected from the group consisting of ginger oil, rosemary oil, clove oil, allspice oil, aniseed oil, lemon oil, orange oil, peppermint oil, evening primrose oil, olive oil, sunflower oil, vitamin E oil, cod liver oil, medium chain triglyceride oil, linseed oil, wheat germ oil, and mixtures thereof.

Preferred oils are sunflower oil, orange oil, evening primrose oil, and lemon oil. The oil may make up between 0.5 % by mass and 25% by mass of the capsule.

The density modifying agent may be a gas trapped within the water insoluble particle-forming encapsulating agent. The gas may be carbon dioxide or air.

When the density modifying agent is carbon dioxide, it may be formed in situ in the capsules, for example, by incorporating a carbon dioxide- generating component, for example a salt such as sodium hydrogen carbonate, in the capsules and bringing the capsules into contact with an acid component such as citric acid which can diffuse through the polymer wall or encapsulating agent into contact with the salt and generate carbon dioxide by reaction between the salt and the acid.

The capsule may have a density of between 0,3 g/cm³ and 2 g/cm³. Typically, the capsule has a density of between 0,9 g/cm³ and 1 ,5 g/cm³.

The water insoluble particle-forming encapsulating agent may be a water insoluble cross-linked polysaccharide such as cross-linked sodium aiginate, cross-linked gellan gum, or cross-linked gelatin. This would typically be the case where the functional ingredient is water insoluble. Such cross- linked polysaccharide capsules are typically porous at least to some extend . Thus, the encapsulating agent may be sodium aiginate which is available from Transarc as "MANUGEL DJX-FOODGRADE". Sodium aiginate capsules may be cross-linked to make them water-insoluble by treatment with a source of divalent ions such as calcium ions, for example, calcium chloride.

The water insoluble particle-forming encapsulating agent may be selected from the group consisting of alginates, ethyl cellulose, methyl ethyl cellulose, methyl cellulose, hydroxy propyl methyl cellulose, gelatine, gum arabic, sodium caseinate, soybean protein, polyvinyl alcohol, starch, carrageenin, albumin, gellan gum, and mixtures thereof, the encapsulating agent having been treated if necessary to ensure that it forms a water insoluble capsule.

In a preferred embodiment of the invention, the water insoluble particle-forming encapsulating agent is selected from the group consisting of sodium aiginate, ethyl cellulose, methyl ethyl cellulose, hydroxy propyl methyl cellulose, and mixtures thereof, the encapsulating agent having been treated (e.g . with a cross-linking agent) if necessary to ensure that it forms a water insoluble capsule.

As mentioned above, the water insoluble particle-forming encapsulating agent is typically cross-linked sodium aiginate or an other cross- linked polysaccharide when the functional ingredient is water insoluble. When the functional ingredient is water soluble, the particle-forming encapsulating agent is typically ethyl cellulose, methyl ethyl cellulose or hydroxy propyl methyl cellulose, which is insoluble in water, unlike sodium aiginate, gellan gum or gelatine which is soluble until it has been cross-linked, and the capsule is then typically further coated or encapsulated with cross-linked sodium aiginate, cross-linked gellan gum, or cross-linked gelatin, to form a more porous capsule as hereinafter described. In this way, when the functional ingredient is water soluble, there is advantageously ensured that no dissolved particle-forming encapsulating agent is present with the functional ingredient in the capsule. When the functional ingredient is water soluble, the capsules may have a particle size in the range 0, 1 - 0,8 mm, more preferably 0,2 - 0,7 mm, and most preferably 0,3 - 0,5 mm. They may be substantially spherical or any other shape, and may be more accurately described as micro capsules when they have the above particle sizes.

According to a second aspect of the invention, there is provided an edible capsule configured to be suspended in a liquid and which includes at least one edible capsule as hereinbefore described; and an edible water insoluble encapsulating coating which encapsulates said at least one capsule.

It is to be appreciated that the terms water insoluble particle- forming encapsulating agent and water insoluble encapsulating coating are used in this specification to distinguish between two materials which may be present in a single capsule, and that both the coating and the agent has the function to encapsulate something . Thus, in fact, the purpose of the encapsulating coating is also to encapsulate, and not merely to coat.

The water insoluble encapsulating coating which encapsulates said at least one capsule may be cross-linked sodium aiginate, cross-linked gellan gum, cross-linked gelatin, or mixtures thereof. Preferably, the water insoluble encapsulating coating is sodium aiginate.

The functional ingredient of said at least one capsule may be water soluble. The water permeability and porosity of the water insoluble encapsulating coating is preferably higher than the water permeability and porosity of the particle-forming encapsulating agent. This advantageously provides a "softer" capsule than said at least one capsule which is encapsulated, which makes the capsule more acceptable when taken into the mouth. It also allows for the capsule to be infiltrated with a liquid such as water when the capsule is suspended in the liquid, thus allowing the density of the capsule to be modified by the liquid . The capsule may encapsulate between 5 and 1 0 of said capsules as hereinbefore described, and may have a particle size in the range of 1 mm to 4 mm, typically 2 mm to 4 mm.

The capsule may have a density of between 0,5 g/cm³ and 2 g/cm³. Typically, the capsule has a density of between 0,8 g/cm³ and 1 ,3 g/cm .

According to a third aspect of the invention, there is provided a beverage having a plurality of edible capsules suspended in a liquid, the capsules including at least one functional ingredient; and a water insoluble particle-forming encapsulating agent which encapsulates the functional ingredient and which inhibits diffusion of the functional ingredient from the capsule into the liquid.

A ratio of the density of the liquid to the density of the capsules, when dry, may range between 1 ,5: 1 and 1 , 1 : 1 . Typically, the ratio of the density of the liquid to the density of the capsules, when dry, ranges between 1 ,2: 1 and 1 , 1 5: 1 . Preferably, when in a state of equilibrium, the capsules have a range of densities such that they are suspended or distributed throughout all depths in the liquid of the beverage.

The beverage may be a soft drink, for example a water-based soft drink. The soft drink may contain additives such as flavour-enhancing agents, taste-enhancing agents such as sugars, preservatives, and the like.

Typically, the liquid is transparent and the capsules are coloured.

The capsules may be as hereinbefore described, or may form part of capsules as hereinbefore described. The capsules may be porous at least to some extent, thus allowing the liquid of the beverage to infiltrate the pores of the capsules to increase the density of the capsules so that their density is very similar to the density of the liquid.

According to a fourth aspect of the invention, there is provided a process for preparing edible capsules having a predetermined density and which are configured to be suspended in a liquid, the process including preparing an admixture capable of forming particles and having a predetermined density, the admixture including at least one edible functional ingredient and an edible encapsulating agent for encapsulating the functional ingredient and which is capable of inhibiting diffusion of the functional ingredient from the capsules, once formed; and treating the admixture to form water insoluble capsules.

The functional ingredient may be as hereinbefore described.

The functional ingredient and the encapsulating agent may be admixed in a ratio such that the capsules formed contain between 0.01 % by mass and 1 0% by mass of the functional ingredient. Typically, the functional ingredient and the encapsulating agent are admixed in a ratio such that the capsules formed contain between 2% by mass and 5% by mass of the functional ingredient.

The encapsulating agent may be as hereinbefore described.

The functional ingredient may be oxidizable. The process may include admixing an antioxidant or an oxygen scavenger with the functional ingredient and the encapsulating agent to inhibit oxidation of the functional ingredient. The process may include admixing at least one density modifying agent with the functional ingredient and the encapsulating agent thereby to modify the density of the capsules formed.

The density modifying agent may be as hereinbefore described, e.g . an oil.

The oil, the functional ingredient and the encapsulating agent may be admixed in a ratio such that the capsules contain between 0.5% by mass and 25% by mass of the oil.

The process may include admixing a carbon dioxide-generating substance with the functional ingredient and the encapsulating agent and, once the capsules have been formed, bringing the capsules into contact with an acid which can diffuse through the encapsulating agent to react with the carbon dioxide-generating substance thereby generating carbon dioxide which is trapped within the capsules.

The carbon dioxide generating substance may be sodium hydrogen carbonate and the acid may be citric acid.

The encapsulating agent may be as hereinbefore described.

The encapsulating agent may be a polysaccharide. Treating the admixture to form capsules may include forming droplets of the admixture and cross-linking the polysaccharide to ensure that it is water insoluble.

Treating the admixture to form capsules may include extruding the admixture to form droplets, and contacting the droplets with a gelling agent.

The encapsulating agent may be sodium aiginate, gellan gum or gelatin, particularly when the functional ingredient is water insoluble. Preferably, the encapsulating agent is sodium aiginate. Treating the admixture to form capsules may then include extruding the admixture to form droplets and contacting the droplets with a gelling agent which includes a divalent ion selected from the group consisting of Mg^{2 +} , Zn^{2 +} , Ca^{2 +} , and mixtures thereof.

The process may include contacting the capsules formed with a sodium citrate solution thereby softening the encapsulating sodium aiginate, reducing the density of the capsules, and increasing the porosity or water permeability of the capsules.

In one embodiment of the invention, particularly when the functional ingredient is water soluble, the encapsulating agent is selected from the group consisting of ethyl cellulose, methyl ethyl cellulose, hydroxy propyl methyl cellulose, and mixtures thereof, in admixture with a solvent for the encapsulating agent. Treating the admixture to form capsules may then include evaporating the solvent. The solvent may be dichloromethane or ethanol.

The invention also extends to a process of making a capsule, which process comprises the steps of dissolving a polymeric material and at least one carbon dioxide- generating component in an aqueous medium at an elevated temperature to form a solution; cooling said solution to ambient temperature; mixing at least one active ingredient with said cooled solution; extruding said active ingredient-containing solution into an aqueous solution containing ions to form water-insoluble cross-linked beads encapsulating the active ingredient and the carbon dioxide-generating component; recovering the beads and drying them; subjecting the dried beads to an aqueous solution of an acid component to permit the acid component to diffuse through the polymer wall of the bead to react with the carbon dioxide-generating component to form sufficient carbon dioxide to control the density of the bead such that the bead can float and/or be suspended in the aqueous solution.

According to a fifth aspect of the invention, there is provided a process for preparing edible capsules having a predetermined density and which are configured to be suspended in a liquid, the process including admixing the capsules prepared in accordance with the process as hereinbefore described with an encapsulating coating; and treating the admixture to form at least some water insoluble capsules each of which encapsulates at least one of said capsules prepared in accordance with the process as hereinbefore described .

The encapsulating coating with which the capsules are admixed may be sodium aiginate, gellan gum or gelatine. Preferably, the encapsulating coating is sodium aiginate. Treating the admixture to form water insoluble capsules may then include extruding the admixture to form droplets and contacting the droplets with a gelling agent which includes a divalent ion selected from the group consisting of Mg^{2 +} , Zn^{2 +} , Ca^{2 +} , and mixtures thereof.

Each capsule may encapsulate between 5 and 10 of the capsules prepared in accordance with the process as hereinbefore described .

Naturally, routine experimentation may be carried out with regard to the various parameters of the invention such as the specific encapsulating agent, coating or polymer, the concentration thereof and the amount of the density modifying agent, to achieve optimum, or at least acceptable, results, bearing practical and economic considerations in mind .

The invention will now be described, by way of example, with reference to the accompanying illustrations and the following non-limiting examples.

In the illustrations,

Figure 1 shows a photograph of a micro analysis of a sectioned capsule containing vitamin-E-acetate prepared in accordance with Example 5 below; Figure 2 shows a photograph of a micro analysis of capsules containing co-enzyme Q10 prepared in accordance with Example 7 below; Figure 3 shows a photograph of a micro analysis of capsules containing Puramex calcium prepared in a similar manner as described in

Example 7 below; Figure 4 shows a photograph of a micro analysis of a capsule encapsulating a plurality of capsules containing L-carnitine L-tartrate prepared in accordance with Example 6 below;

Figure 5 shows a photograph of a micro analysis of capsules containing Siberian ginseng extract prepared in a similar manner as described in Example 7 below.

EXAMPLE 1

Step 1

Sodium aiginate available from Transarc as "MANUGEL DJX-

FOODGRADE" (2.5g) , sodium citrate (preservative) (0.8g), sodium hydrogen carbonate (CO₂ generator) (2g) and distilled water (97, 5g) were heated together at 60°C for 60 minutes until completely dissolved. The solution was then allowed to cool to room temperature. Step 2

The solution prepared in Step 1 (20g), creatine (active ingredient) and a food pigment in the form of iron oxide pigments available from BASF as "SICOVIT GELB 10E 1 72" were mixed well together.

Step 3

The solution prepared in Step 2 was extruded into 1 - 5% calcium chloride solution (the exact concentration depending on the amount of cross- linking required) to form cross-linked water-insoluble beads or capsules. The beads were then removed from the solution and rinsed .

Step 4

The rinsed beads were then put into 10% citric acid solution and left in the solution until sufficient CO2 was generated within the beads (by the diffusion of the citric acid through the sodium aiginate wall and reaction with the sodium hydrogen carbonate) thereby controlling the density of the beads to permit the beads to float or be suspended in the solution.

Step 5

The beads were removed from the citric acid solution and rinsed . The beads were water-insoluble and spherical having a size of 1 - 2 mm in diameter.

Step 6

A plurality of the beads from Step 5 were added to a transparent soft drink to form the beverage of the invention.

It should be noted that the amount of sodium aiginate employed in Step

1 may be varied between 1 % and 3% depending on the size of the beads required. Also, the amount of sodium hydrogen carbonate used may be varied to control the amount of CO2 generated and therefore control the density of the beads formed. EXAMPLE 2

In this example, oil based systems are used to control the density of the beads or capsules. The oil can be used from 0.5 - 25 % .

Sodium aiginate available from Transarc as "MANUGEL DJX- FOODGRADE" ( 1 g), sodium citrate ( 1 g) and Xanthan gum (0.05g) were combined and stirred in 85g of distilled water at 60°C for 30 minutes, or until all the sodium aiginate and Xanthan gum had dissolved . Evening primrose oil (5g) , iron oxide pigment (SICOVIT GELB 1 0E 1 72 from BASF) (0.05g), an oil- based fruit flavourant (supplied by Nicola J) (2.5g) and lectin (emulsifying agent) (0.03g) were added to the solution as well as creatine (5g) . The mixture was then thoroughly mixed and extruded into a 1 % calcium chloride solution.

The resulting capsules were then removed from the salt solution and washed with distilled water.

EXAMPLE 3

Different oils of different density were suspended in different concentrations of sodium aiginate (viscosity 1 90 - 200 cps) as in Table 1 and pigment was added to the mixtures with stirring. The mixtures of oil and sodium aiginate were extruded through a plastic pipette, in order to produce micro droplets, into a 1 ,5% w/w CaC^ solution to form gelled micro capsules containing the different oils. The residence time of the capsules in the CaC^ solution was less than 2 minutes. The capsules were filtered off using a sieve and suspended in a 1 ,5% w/w Na-citrate solution for 1 , 2 or 3 minute intervals as a means to modify the density of the capsules. The capsules were filtered off, and washed well with a 2% w/w NaCI solution, where after they were stored in a soft drink composition. Table 1 : Oil and vitamin

EXAMPLE 4

Vitamin-E-acetate (Abl: 42 - 1 241 ) 2% w/w and an antioxidant (butylated hydroxy toluene) were added together to a solution of 1 ,5% w/w Na-alginate. A water-insoluble pigment Abl-Nr 43 091 5 Indigotin was added to the mixture. The mixture was extruded through a plastic pipette producing micro droplets into a 1 ,5% CaC^ solution to form gelled vitamin-E-acetate micro capsules. The residence time of the capsules in the CaC^ was less than 2 minutes. The capsules were filtered and suspended in a 1 ,5% w/w Na-citrate solution for less than 1 ,5 minutes. The capsules were filtered and washed well with a 2% w/w NaCI solution. The vitamin-E-acetate-containing capsules were then stored in a soft drink composition.

EXAMPLE 5

Vitamin-E-acetate 22,40g and an antioxidant (butylated hydroxy toluene) 0,466g were added to a solution of ethyl cellulose N7 01 00 (46,70g) in 200 m£ dichloromethane. A yellow pigment Indigotin Abl-Nr 43-091 5 was added. The solution was added with stirring to a 2% w/w aqueous solution of Tween 80 in a one liter beaker. The mixture was stirred overnight until the dichloromethane had evaporated. The capsules formed were filtered off, washed with water and dried in a fluidized bed with a drying temperature of 30°C, a 1 bar atomizer and a drying time of 30 minutes. The dry capsules were suspended in a 1 ,5% Na-alginate solution (viscosity 1 85 cps) and extruded through a plastic pipette producing micro droplets into a 1 ,5 % w/w CaC^ solution to form transparent gelled vitamin-containing capsules through which the yellow vitamin-E-acetate containing capsules were visible. The capsules were suspended in a 1 ,5 % w/w Na-citrate solution for 1 ,5 minutes and filtered . The capsules were then washed well with 2% w/w Nail and stored in a soft drink composition.

EXAMPLE 6

L-Carnitine L-tartrate is mostly used in sport nutrition to provide nutritional support for producing energy in muscles and the heart and at the same time raise energy, endurance and stamina during heavy exercise.

A wet homogeneous mixture was obtained by mixing 100 g of hydroxy propyl methyl cellulose and 50 g of L-Carnitine L-tartrate with 50 ml of distilled water for 20 minutes. The mixture was extruded in a Niro-filder extruder E-140 using a die of diameter 0,5 mm. The temperature was controlled throughout the process by regulating the feeder/impeller speed. The extrusion time was 14 minutes, the temperature was 23 °C, and the feeder and impeller speeds 35 and 20 rpm respectively.

The extrudates were then spheronized to form micro capsules using an Aeromatic-Fielder Spheroniser S-320. The speed was regulated throughout the process at 900 rpm for 30 minutes. The capsules were dried in an oven for one hour at a temperature of 75 °C.

1 0 g of the capsules were mixed with a 1 .5 % w/w sodium aiginate solution and extruded into a calcium chloride solution. The residence time in the calcium chloride solution was 2 minutes.

The resultant capsules were suspended in a 2 % w/w sodium citrate solution for a maximum of 2 minutes and later washed with a 1 % w/w sodium chloride solution. The capsules were suspended in a soft drink solution and the stability of the capsules was monitored for thirty days. No stability problems were noticed.

EXAMPLE 7

In the encapsulation of co-enzyme, Q10 oil based systems were used to control the density of the capsules. In this case, rosemary oil was used.

A 2 % w/w sodium aiginate and 1 % w/w rosemary oil admixture was prepared by thoroughly mixing the sodium aiginate and the rosemary oil together using a magnetic stirrer at a temperature of 25 °C. 5 g of co- enzyme Q1 0 was dispersed in 50 ml of the resultant admixture and mixed for

45 minutes.

The resultant admixture was extruded through a 1 ,5 % calcium chloride solution. The resident time in the calcium chloride solution was 2 minutes.

Other biologically active ingredients that were successfully encapsulated include zinc-L-2-hydroxy propionate (Puramex Zn), Mg-L-2- hydroxy-propionate (Puramex Mg) , and Ca-L-2-hydroxy-propionate (Puramex Ca) .

It is an advantage of the invention that it provides means for delivering or administering vitamins or the like to a person, for example a child, who may resist or refuse to take the vitamins (or possible medicines) when administered or delivered by conventional means. The beverage may also serve as a sports or health drink with novelty attraction.

Claims

CLAIMS:

1 . An edible capsule having a predetermined density and which is configured to be suspended in a liquid, the capsule including at least one edible functional ingredient; and an edible water insoluble particle-forming encapsulating agent which encapsulates the functional ingredient and which inhibits diffusion of the functional ingredient from the capsule.

2. A capsule as claimed in claim 1 , in which the functional ingredient is a food grade pigment.

3. A capsule as claimed in claim 1 , in which the functional ingredient is a biologically active ingredient.

4. A capsule as claimed in claim 3, in which the biologically active ingredient is selected from the group consisting of energy source materials, amino acids, vitamins, creative homeopathic remedies, electrolytes, minerals, trace minerals, medicaments, enzymes, herbal extracts, muscle-builders, appetite suppressants, performance enhancement substances, and mixtures thereof.

5. A capsule as claimed in claim 4, in which the active ingredient is an energy source material which is selected from the group consisting of sugars, starches, simple carbohydrates, xylitols, artificial sweeteners, and mixtures thereof.

6. A capsule as claimed in claim 4, in which the active ingredient is a mineral selected from the group consisting of iron, magnesium, fluoride, calcium, phosphorus, manganese, iodine, copper, zinc, potassium, selenium, chromium, and mixtures thereof.

7. A capsule as claimed in claim 4, in which the active ingredient is a trace mineral selected from the group consisting of selenium, zinc, and mixtures thereof.

8. A capsule as claimed in any one of the preceding claims, which contains between 0.01 % by mass and 10% by mass of the functional ingredient.

9. A capsule as claimed in claim 8, which contains between 2% by mass and 5% by mass of the functional ingredient.

1 0. A capsule as claimed in any one of the preceding claims, in which the water insoluble particle-forming encapsulating agent is a material which is biodegradable or biocompatible.

1 1 . A capsule as claimed in any one of the preceding claims, in which the functional ingredient is oxidizable, the capsule including an antioxidant or an oxygen scavenger to inhibit oxidation of the functional ingredient.

1 2. A capsule as claimed in any one of the preceding claims, which includes at least one density modifying agent which modifies the density of the capsule to a predetermined extend thereby permitting the capsule to be suspended in a preselected liquid of particular density.

1 3. A capsule as claimed in claim 1 2, in which the density modifying agent is an oil.

1 4. A capsule as claimed in claim 1 3, in which the oil is selected from the group consisting of ginger oil, rosemary oil, clove oil, allspice oil, aniseed oil, lemon oil, orange oil, peppermint oil, evening primrose oil, olive oil, sunflower oil, vitamin E oil, cod liver oil, medium chain triglyceride oil, linseed oil, wheat germ oil, and mixtures thereof.

1 5. A capsule as claimed in claim 14, in which the oil makes up between 0.5 % by mass and 25% by mass of the capsule.

1 6. A capsule as claimed in claim 1 2, in which the density modifying agent is a gas trapped within the water insoluble particle-forming encapsulating agent.

1 7. A capsule as claimed in claim 1 6, in which the gas is carbon dioxide.

1 8. A capsule as claimed in any one of the preceding claims, which has a density of between 0,3 g/cm° and 2 g/cm .

1 9. A capsule as claimed in claim 1 8, which has a density of q q between 0,9 g/crrr and 1 ,5 g/cm .

20. A capsule as claimed in any one of the preceding claims, in which the water insoluble particle-forming encapsulating agent is a water insoluble cross-linked polysaccharide.

21 . A capsule as claimed in any one of claims 1 to 1 9 inclusive, in which the water insoluble particle-forming encapsulating agent is selected from the group consisting of alginates, ethyl cellulose, methyl ethyl cellulose, methyl cellulose, hydroxy propyl methyl cellulose, gelatine, gum arabic, sodium caseinate, soybean protein, polyvinyl alcohol, starch, carrageenin, albumin, gellan gum, and mixtures thereof, the encapsulating agent having been treated if necessary to ensure that it forms a water insoluble capsule.

22. A capsule as claimed in any one of claims 1 to 1 9 inclusive, in which the water insoluble particle-forming encapsulating agent is selected from the group consisting of sodium aiginate, ethyl cellulose, methyl ethyl cellulose, hydroxy propyl methyl cellulose, and mixtures thereof, the encapsulating agent having been treated if necessary to ensure that it forms a water insoluble capsule.

23. An edible capsule configured to be suspended in a liquid and which includes at least one edible capsule as claimed in any one of claims 1 to 1 9; and an edible water insoluble encapsulating coating which encapsulates said at least one capsule.

24. A capsule as claimed in claim 23, in which the functional ingredient is water insoluble and the water insoluble particle-forming encapsulating agent of said at least one encapsulated capsule is a water insoluble cross-linked polysaccharide.

25. A capsule as claimed in claim 23, in which the water insoluble particle-forming encapsulating agent of said at least one encapsulated capsule is selected from the group consisting of alginates, ethyl cellulose, methyl ethyl cellulose, methyl cellulose, hydroxy propyl methyl cellulose, gelatine, gum arabic, sodium caseinate, soybean protein, polyvinyl alcohol, starch, carrageenin, albumin, gellan gum, and mixtures thereof, the encapsulating agent having been treated if necessary to ensure that it forms a water insoluble capsule.

26. A capsule as claimed in claim 23, in which the functional ingredient is water soluble and the water insoluble particle-forming encapsulating agent of said at least one encapsulated capsule is selected from the group consisting of ethyl cellulose, methyl ethyl cellulose, hydroxy propyl methyl cellulose, and mixtures thereof, the encapsulating agent having been treated if necessary to ensure that it forms a water insoluble capsule.

27. A capsule as claimed in any one of claims 23 to 26 inclusive, in which the water insoluble encapsulating coating which encapsulates said at least one capsule is selected from the group consisting of cross-linked sodium aiginate, cross-linked gellan gum, cross-linked gelatine, or mixtures thereof.

28. A capsule as claimed in claim 23 or claim 26, in which the water permeability of the water insoluble encapsulating coating is higher than the water permeability of the water insoluble particle-forming encapsulating agent.

29. A capsule as claimed in any one of claims 23 to 28 inclusive, which encapsulates between 5 and 1 0 of the capsules as claimed in any one of claims 1 to 1 9, inclusive.

30. A capsule as claimed in any one of claims 23 to 29 inclusive,

3 which has a density of between 0,5 g/crrr and 2 g/cm .

31 . A capsule as claimed in claim 30, which has a density of q q between 0,8 g/crrr and 1 ,3 g/crrr.

32. A beverage having a plurality of edible capsules suspended in a liquid, the capsules including at least one functional ingredient; and a water insoluble particle-forming encapsulating agent which encapsulates the functional ingredient and which inhibits diffusion of the functional ingredient from the capsule into the liquid.

33. A beverage as claimed in claim 32, in which a ratio of the density of the liquid to the density of the capsules, when dry, ranges between 1 ,5: 1 and 1 , 1 : 1 .

34. A beverage as claimed in claim 33, in which the ratio of the density of the liquid to the density of the capsules, when dry, ranges between 1 ,2: 1 and 1 , 1 5: 1 .

35. A beverage as claimed in any one of claims 32 to 34 inclusive, which is a water-based soft drink.

36. A beverage as claimed in any one of claims 32 to 35 inclusive, in which the liquid is transparent and in which the capsules are coloured .

37. A beverage as claimed in any one of claims 32 to 36 inclusive, in which the capsules are as claimed in any one of claims 1 to 22 inclusive.

38. A beverage as claimed in claim 37, in which the capsules form part of capsules as claimed in any one of claims 23 to 31 inclusive.

39. A beverage as claimed in any one of claims 32 to 38 inclusive, in which the capsules are porous at least to some extent, thus allowing the liquid of the beverage to infiltrate the pores of the capsules to increase the density of the capsules so that their density is very similar to the density of the liquid .

40. A beverage as claimed in any one of claims 32 to 39 inclusive, in which, when in a state of equilibrium, the capsules have a range of densities such that they are suspended or distributed throughout all depths in the liquid of the beverage.

41 . A process for preparing edible capsules having a predetermined density and which are configured to be suspended in a liquid, the process including preparing an admixture capable of forming particles and having a predetermined density, the admixture including at least one edible functional ingredient and an edible encapsulating agent for encapsulating the functional ingredient and which is capable of inhibiting diffusion of the functional ingredient from the capsules, once formed; and treating the admixture to form water insoluble capsules.

42. A process as claimed in claim 41 , in which the functional ingredient is a food grade pigment.

43. A process as claimed in claim 41 , in which the functional ingredient is a biologically active ingredient.

44. A process as claimed in claim 43, in which the biologically active ingredient is selected from the group consisting of energy source materials, amino acids, vitamins, creative homeopathic remedies, electrolytes, minerals, trace minerals, medicaments, enzymes, herbal extracts, muscle-builders, appetite suppressants, performance enhancement substances, and mixtures thereof.

45. A process as claimed in claim 44, in which the biologically active ingredient is an energy source material which is selected from the group consisting of sugars, starches, simple carbohydrates, xylitols, artificial sweeteners, and mixtures thereof.

46. A process as claimed in claim 44, in which the biologically active ingredient is a mineral selected from the group consisting of iron, magnesium, fluoride, calcium, phosphorus, manganese, iodine, copper, zinc, potassium, selenium, chromium, and mixtures thereof.

47. A process as claimed in claim 44, in which the biologically active ingredient is a trace mineral selected from the group consisting of selenium, zinc, and mixtures thereof.

48. A process as claimed in any one of claims 41 to 47 inclusive, in which the functional ingredient and the encapsulating agent are admixed in a ratio such that the capsules formed contain between 0.01 % by mass and 10% by mass of the functional ingredient.

49. A process as claimed in claim 48, in which the functional ingredient and the encapsulating agent are admixed in a ratio such that the capsules formed contain between 2% by mass and 5 % by mass of the functional ingredient.

50. A process as claimed in any one of claims 41 to 49 inclusive, in which the encapsulating agent is a material which is biodegradable or biocompatible.

51 . A process as claimed in any one of claims 41 to 50 inclusive, in which the functional ingredient is oxidizable, the process including admixing an antioxidant or an oxygen scavenger with the functional ingredient and the encapsulating agent to inhibit oxidation of the functional ingredient.

52. A process as claimed in any one of claims 41 to 51 inclusive, which includes admixing at least one density modifying agent with the functional ingredient and the encapsulating agent thereby to modify the density of the capsules formed.

53. A process as claimed in claim 52, in which the density modifying agent is an oil.

54. A process as claimed in claim 53, in which the oil is selected from the group consisting of ginger oil, rosemary oil, clove oil, allspice oil, aniseed oil, lemon oil, orange oil, peppermint oil, evening primrose oil, olive oil, sunflower oil, vitamin E oil, cod liver oil, medium chain triglyceride oil, linseed oil, wheat germ oil, and mixtures thereof.

55. A process as claimed in claim 52 or claim 53, in which the oil, the functional ingredient and the encapsulating agent are admixed in a ratio such that the capsules contain between 0.5% by mass and 25% by mass of the oil.

56. A process as claimed in any one of claims 41 to 51 inclusive, which includes admixing a carbon dioxide-generating substance with the functional ingredient and the encapsulating agent and, once the capsules have been formed, bringing the capsules into contact with an acid which can diffuse through the encapsulating agent to react with the carbon dioxide- generating substance thereby generating carbon dioxide which is trapped within the capsules.

57. A process as claimed in claim 56, in which the carbon dioxide generating substance is sodium hydrogen carbonate and the acid is citric acid.

58. A process as claimed in any one of claims 41 to 57 inclusive, in which the encapsulating agent is a polysaccharide, and in which treating the admixture to form capsules includes forming droplets of the admixture and cross-linking the polysaccharide to ensure that it is water insoluble.

59. A process as claimed in any one of claims 41 to 57 inclusive, in which the encapsulating agent is selected from the group consisting of alginates, ethyl cellulose, methyl ethyl cellulose, methyl cellulose, hydroxy propyl methyl cellulose, gelatine, gum arabic, sodium caseinate, soybean protein, polyvinyl alcohol, starch, carrageenin, albumin, gellan gum, and mixtures thereof, the encapsulating agent having been treated if necessary to ensure that it forms a water insoluble capsule.

60. A process as claimed in any one of claims 41 to 57 inclusive, in which the encapsulating agent is selected from the group consisting of sodium aiginate, ethyl cellulose, methyl ethyl cellulose, hydroxy propyl methyl cellulose, and mixtures thereof.

61 . A process as claimed in claim 59 or claim 60, in which treating the admixture to form capsules includes extruding the admixture to form droplets, and contacting the droplets with a gelling agent.

62. A process as claimed in any one of claims 41 to 57 inclusive, in which the encapsulating agent is sodium aiginate, and in which treating the admixture to form capsules includes extruding the admixture to form droplets and contacting the droplets with a gelling agent which includes a divalent ion selected from the group consisting of Mg^{2 +} , Zn^{2 +} , Ca^{2 +} , and mixtures thereof.

63. A process as claimed in claim 62, which includes contacting the capsules formed with a sodium citrate solution thereby softening the encapsulating sodium aiginate and reducing the density of the capsules.

64. A process as claimed in any one of claims 41 to 57 inclusive, in which the encapsulating agent is selected from the group consisting of ethyl cellulose, methyl ethyl cellulose, hydroxy propyl methyl cellulose, and mixtures thereof, in admixture with a solvent for the encapsulating agent, and in which treating the admixture to form capsules includes evaporating the solvent.

65. A process as claimed in claim 64, in which the solvent is dichloromethane or ethanol.

66. A process for preparing edible capsules having a predetermined density and which are configured to be suspended in a liquid, the process including admixing the capsules prepared in accordance with the process as claimed in any one of claims 41 to 57 with an encapsulating coating; and treating the admixture to form at least some water insoluble capsules each of which encapsulates at least one of said capsules prepared in accordance with the process as claimed in any one of claims 41 to 57.

67. A process as claimed in claim 66, in which the encapsulating agent of said capsules is selected from the group consisting of alginates, ethyl cellulose, methyl ethyl cellulose, methyl cellulose, hydroxy propyl methyl cellulose, gelatine, gum arabic, sodium caseinate, soybean protein, polyvinyl alcohol, starch, carrageenin, albumin, gellan gum, and mixtures thereof, the encapsulating agent having been treated if necessary to ensure that it forms a water insoluble capsule.

68. A process as claimed in claim 66, in which the encapsulating agent of said capsules is selected from the group consisting of ethyl cellulose, methyl ethyl cellulose, hydroxy propyl methyl cellulose, and mixtures thereof.

69. A process as claimed in any one of claims 66 to 68 inclusive, in which the encapsulating coating with which said capsules are admixed is sodium aiginate, and in which treating the admixture to form water insoluble capsules includes extruding the admixture to form droplets and contacting the droplets with a gelling agent which includes a divalent ion selected from the group consisting of Mg ⁺ , Zn ⁺ , Ca ⁺ , and mixtures thereof.

70. A process as claimed in claim 69, which includes contacting the capsules formed with a sodium citrate solution thereby softening the encapsulating sodium aiginate and reducing the density of the capsules.

71 . A process as claimed in any one of claims 66 to 70 inclusive, in which the functional ingredient of said capsules is water soluble.

72. A process as claimed in any one of claims 66 to 71 inclusive, in which each capsule encapsulates between 5 and 10 of said capsules.

73. A capsule as claimed in claim 1 , substantially as herein described and illustrated.

74. A capsule as claimed in claim 23, substantially as herein described and illustrated.

75. A beverage as claimed in claim 32, substantially as herein described and illustrated .

76. A process as claimed in claim 41 or claim 66, substantially as herein described and illustrated .

77. A new capsule; or a new process for preparing a capsule; or a new beverage, substantially as herein described.