Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients

• US 8,911,783 B2
• Filed: 09/17/2010
• Issued: 12/16/2014
• Est. Priority Date: 12/18/2003
• Status: Active Grant

• Current Assignee: Chemische Fabrik Budenheim KG (Dr August Oetker KG)
• Original Assignee: Victor Casana Giner
• Inventors: Casaa Giner, Victor, Gimeno Sierra, Miguel, Gimeno Sierra, Barbara, Moser, Martha
• Primary Examiner(s): Hartley, Michael G
• Assistant Examiner(s): YOUNG, MICAH PAUL
• Application Number:
  US12/885,108
• Publication Number:
  US 20110064817A1
• Time in Patent Office: 1,551 Days
• Field of Search: 424464-489
• US Class Current: 424/489
• CPC Class Codes: A61P 25/00 Drugs for disorders of the nervous system
• CPC Class Codes: B01J 13/18 In situ polymerisation with all reactants being present in the same phase

Abstract

The invention relates to microcapsules, and a continuous micro-encapsulation water-in-oil-in-water microencapsulation process through in situ and interfacial polymerization of the emulsion. The formulation comprises a continuous water phase having a dispersion of microcapsules which contain oil drops and wherein the inside of each oil phase drop—containing optionally oil-soluble materials—there is a dispersion of water, or aqueous extract or water dispersible material or water soluble material. The oil drops are encapsulated with a polymerizable material of natural origin. Such microcapsules are appropriated for spray-dry processes, to be used as dry powder, lyophilized, self-emulsifiable powder, gel, cream and any liquid form. The active compounds included in the microcapsules are beneficial to the health and other biological purposes. Such formulations are appropriate to be incorporated in any class of food, especially for the production of nutraceuticals, as well as cosmetic products (such as rejuvenescence creams, anti-wrinkle creams, gels, bath and shower consumable products and sprays). The preparations are adequate to stabilize compounds added to the food, media for cultivating microbes and nutraceuticals, especially those which are easily degradable or oxidizable.

Claims

1. A method comprising:

(a) preparing microcapsules of at least one biologically active ingredient(s) comprising an anabolite or nutrient, comprising;

(i) forming a water in oil emulsion comprising a water phase, an oil phase, a polymerization initiator, an emulsifier and the at least one biologically active ingredient(s), wherein;

the polymerization initiator exists in the water phase,

the emulsifier exists in the oil phase or in the water phase,

the biologically active ingredient(s) exists in the oil phase and/or in the water phase;

(ii) adding an aqueous solution or dispersion containing at least one hydrocolloid(s) which is polymerizable due to the polymerization initiator and thereby producing a phase inversion whereby there are drops of water in oil and polymerization and cross-linking of the hydrocolloid(s) onto the drops of water in oil;

(iii) adding an aqueous solution or dispersion containing at least one protective colloid(s) and thereby depositing the protective colloid(s) on the surface of the drops of water in oil, whereby the protective colloid(s) polymerizes and cross-links with itself and the hydrocolloid(s);

(iv) adding an aqueous solution or dispersion containing a surfactant and thereby reducing the size of the water in oil drops, whereby microcapsules or multi-microcapsules having a wall and suspended in water result; and

(v) subjecting the microcapsules or multi-microcapsules having a wall and suspended in water to a temperature increase to strengthen the wall,

whereby microcapsules comprising an anabolite or nutrient results from the preparation; and

(b) providing the microcapsules comprising an anabolite or nutrient for contacting with a microbiological culture.

2. The method of claim 1 further comprising contacting the microcapsules with a microbiological culture, whereby the anabolite or nutrient are released from the microcapsules at a constant or quasi-constant rate.

5. The method of any one of claims 1-4 wherein the average particle size of each of the microcapsules 1-10 μ

m.

3. A method comprising:

(a) preparing microcapsules of at least one ingredient(s), comprising;

(i) forming a water in oil emulsion comprising a water phase, an oil phase, a polymerization initiator, an emulsifier and the at least one ingredient(s), wherein;

the polymerization initiator exists in the water phase,

the emulsifier exists in the oil phase or in the water phase,

the ingredient(s) exists in the oil phase and/or in the water phase;

(ii) adding an aqueous solution or dispersion containing at least one hydrocolloid(s) which is polymerizable due to the polymerization initiator and thereby producing a phase inversion whereby there are drops of water in oil and polymerization and cross-linking of the hydrocolloid(s) onto the drops of water in oil;

(iii) adding an aqueous solution or dispersion containing at least one protective colloid(s) and thereby depositing the protective colloid(s) on the surface of the drops of water in oil, whereby the protective colloid(s) polymerizes and cross-links with itself and the hydrocolloid(s);

(iv) adding an aqueous solution or dispersion containing a surfactant and thereby reducing the size of the water in oil drops, whereby microcapsules or multi-microcapsules having a wall and suspended in water result; and

(v) subjecting the microcapsules or multi-microcapsules having a wall and suspended in water to a temperature increase to strengthen the wall,

whereby microcapsules comprising at least one ingredient(s) results from the preparation; and

(b) formulating a composition for ingestion by an individual comprising the microcapsules comprising at least one ingredient(s).

4. The method of claim 3 further comprising the individual ingesting the composition.

7. The method of any one of claim 3, 4, or 6, wherein the composition comprises a natural sweetener, a synthetic sweetener, salt, pepper, a spice or other condiment.

8. The method of any one of claim 3, 4, or 6, wherein the composition is a foodstuff for an animal.

9. The method of claim 8, wherein the animal is one or more members of the group consisting of cattle, fish and domestic pets.

10. The method of any one of claim 3, 4, or 6, wherein the composition is a dry formulation of microcapsules.

11. The method of claim 10 wherein the composition is a human foodstuff or an animal foodstuff.

12. The method of any one of claim 3, 4, or 6, wherein the composition is a foodstuff and the microcapsules contain a mixture of omega-3, omega-6, omega-9, and/or sphingolipids plus a stabilizer selected from vitamin E, vitamin C or ascorbyl palmitate.

13. The method of any one of claim 3, 4, or 6, wherein the microcapsules contain omega-3, omega-6, omega-9, or cerebrosides.

14. The method of any one of claim 3, 4, or 6, wherein the composition comprises a cereal, muesli, a pastry product, a dairy product, a nutritional supplement, a sugar, chocolate, sweets, a nougat, marzipan, a dietary food, a foods for a diabetic, an oil, egg, a vegetable, a fruit, a tuber, an edible shaft, a snack, an appetizer, an edible root, licorice, bay, wild fruit, dried fruit, meat, sausage, fish, shellfish, a crustacean, an alcoholic or non-alcoholic drink, a carbonated or noncarbonated drink, juice, syrup, nectar, spice, condiment, pre-cooked food, preprocessed food, frozen mass of bread, pizza, or honey.

15. The method of any one of claim 3, 4, or 6, wherein at least one of the one or more active ingredients is used in radiology, seeds for radiotherapy, thermotherapy or therapy with light of any wavelength.

16. The method of any one of claim 3, 4, or 6, wherein the microcapsules provide for controlled release therefrom of at least one ingredient from the microcapsules at the pH of a human'"'"'s stomach.

17. The method of any one of claim 3, 4, or 6, wherein the microcapsules contain vectors containing genes.

6. A method comprising:

an individual ingesting a composition comprising microcapsules, each of the microcapsules having a wall containing an inner content of the microcapsules, wherein;

the wall of each of the microcapsules is formed by at least two polymerized hydrocolloids,

the inner content of the microcapsules comprises a first emulsion of water in oil and first inner microcapsules suspended in the first emulsion, wherein there are at least 5 degrees of multi-microencapsulation and each degree of multi-microencapsulation comprises a first microcapsule suspended in an emulsion of water in oil of a second microcapsule,

the average particle size of each of the microcapsules is 1-10 μ

m,

one or more ingredients is present in at least a discontinuous oil phase and/or in a discontinuous water phase in the microcapsules,

the first inner microcapsules each having a wall formed by the at least two polymerized hydrocolloids, and

the inner content of the first inner microcapsules each comprising a second emulsion of water in oil.

18. A method comprising:

contacting microcapsules comprising an anabolite or nutrient with a microbiological culture, whereby the anabolite or nutrient are released from the microcapsules at a constant or quasi-constant rate, wherein;

each of the microcapsules has a wall containing an inner content of the microcapsules,

the wall of each of the microcapsules is formed by at least two polymerized hydrocolloids,

the inner content of the microcapsules comprises a first emulsion of water in oil and first inner microcapsules suspended in the first emulsion, wherein there are at least 5 degrees of multi-microencapsulation and each degree of multi-microencapsulation comprises a first microcapsule suspended in an emulsion of water in oil of a second microcapsule,

the average particle size of each of the microcapsules is 1-10 μ

m, and

the anabolite or nutrient is present in at least a discontinuous oil phase and/or in a discontinuous water phase in the microcapsules.