# US 9,277,759 B2 · Method for manufacturing capsule series, and related capsule series

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- Number: US 9,277,759 B2
- Document ID: US9277759B2
- Status: Granted
- Kind: B2
- Application number: 13/131,971
- Filed: 2009-12-01
- Published: 2012-01-05
- Granted: 2016-03-08
- Earliest claimed: 2008-12-01
- Assignees: Capsum
- Applicants: Jérôme Bibette; Liang-yin Chu; Enric Santanach Carreras; Audrey Royere; Nicolas Bremond
- Inventors: Jérôme Bibette; Liang-yin Chu; Enric Santanach Carreras; Audrey Royere; Nicolas Bremond
- Web page: https://patentgrep.com/patent/US9277759B2

## CPC

- A23P 10/30: Encapsulation of particles, e.g. foodstuff additives
- A23L 27/72: {Encapsulation}
- A61K 8/11: Encapsulated compositions
- A61K 9/4816: {Wall or shell material}
- A61K 9/4833: {Encapsulating processes; Filling of capsules (mechanical aspects A61J3/07)}
- A61P 7/00: Drugs for disorders of the blood or the extracellular fluid
- A61P 29/00: Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
- A61P 31/00: Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P 31/10: Antimycotics
- A61P 33/00: Antiparasitic agents
- A61P 35/00: Antineoplastic agents
- A61Q 19/00: Preparations for care of the skin
- A23P: SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23L: FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF (preservation thereof A23B)
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A61P: SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS

## Abstract

A method includes separately conveying a first liquid solution (36) containing the first material and a second liquid solution (46) containing a liquid polyelectrolyte. The method includes forming of a series of drops (78) at the outlet (50), each drop (78) including a central core (80) formed from a first solution (36) and a peripheral film (82) formed from a second solution. The method includes immersing each drop (78) in a gelling solution (70) containing a reagent capable of reacting with the polyelectrolyte of the film (82) so as to form the gelled casing. The second solution (40) contains at least one surfactant before the former contacts the first solution (36).

## Claims

### Claim 1

A method for manufacturing a capsule series (10), each capsule (10) comprising a liquid core (12) containing at least one first product and a gelled casing (14) completely encapsulating the core (12), the method comprising the following steps:
separately conveying, in a double casing (32), a first liquid solution (36) containing the first product and a second liquid solution (40) containing a liquid polyelectrolyte able to gel ;
forming, at the outlet (50) of the double casing (32), a series of drops (78), each drop (78) comprising a central core (80) formed from the first solution (36) and a peripheral film (82) formed from the second solution and completely covering the central core (80);
immersing each drop (78) in a gelling solution (70) containing a reagent able to react with the polyelectrolyte of the film (82) to make it go from a liquid state to a gelled state and form the gelled casing (14), the central core (80) forming the liquid core (12), wherein the drops (78) formed by co-extrusion in the double casing (32) fall by gravity through a volume of air into the gelling solution (70);
recovering the capsules (10) formed;
wherein the second solution (40) contains at least one surfactant before the former contacts the first solution (36); and
wherein the flow rate of the second solution (40) is comprised between 0.005 times and 0.2 times the flow rate of the first solution (36) at the outlet of the double casing (32).

### Claim 2 (depends on 1)

The method according to claim 1, wherein the or each surfactant is chosen among an anionic surfactant, a cationic surfactant, a non-ionic surfactant, or mixtures thereof.

### Claim 3 (depends on 2)

The method according to claim 2, wherein the surfactant is chosen from among an alkyl sulfate, an alkyl sulfonate, an alkyl aryl sulfonate, an alkaline alkyl phosphate, a dialkyl sulfosuccinate, a salt of saturated or unsaturated alkaline earth fatty acids, a salt of alkylpyridinium or alkylammonium halide such as n-ethyl-dodecylammonium chloride or bromide, cetylammonium chloride or bromide, polyoxyethylenated and/or polyoxypropylenated derivatives of fatty alcohols, fatty acids, or alkylphenols, or among arylphenols, alkyl glucosides, polysorbates, cocamides, or mixtures thereof.

### Claim 4 (depends on 3)

The method according to claim 3, wherein the total weight percentage of surfactant in the second solution (40) is greater than 0.01%.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the or each polyelectrolyte is a polyelectrolyte reactive to multivalent ions.

### Claim 6 (depends on 5)

The method according to claim 5, wherein the ion-reactive polyelectrolyte is an alginate alkaline.

### Claim 7 (depends on 5)

The method according to claim 5, wherein the weight percentage of polyelectrolyte in the second solution (40) is less than 5%.

### Claim 8 (depends on 1)

The method according to claim 1, wherein the first solution comprises (36) at least one of a biologically active product, a cosmetic product, or a comestible product suitable for consumption.

### Claim 9

A capsule series (10), each capsule (10) comprising a liquid core (12) containing at least one first product, and a gelled casing (14) completely encapsulating the liquid core (12) at the periphery thereof, the gelled casing (14) being able to retain the liquid core (12) when the capsule (10) is submerged in a gas, the gelled casing (14) comprising at least one gelled polyelectrolyte;
wherein the gelled casing (14) also comprises at least one surfactant; and
wherein the gelled casing (14) has a thickness between 0.1% and 10% of the diameter of the capsule (10).

### Claim 10 (depends on 6)

The method according to claim 6, wherein the weight percentage of polyelectrolyte in the second solution (40) is less than 5%.

### Claim 11 (depends on 1)

The method according to claim 1, wherein the ratio of the flow rate of the first solution (36) to the flow rate of the second solution (40) at the outlet of the double casing (32) is between 10 and 200.

### Claim 12 (depends on 1)

The method according to claim 1, wherein the gelled casing (14) has a thickness between 0.1% and 2% of the diameter of the capsule (10).

### Claim 13 (depends on 3)

The method according to claim 3, wherein the total weight percentage of surfactant in the second solution (40) is between 0.01% and 0.5%.

### Claim 14 (depends on 1)

The method according to claim 1, wherein the or each polyelectrolyte is a polysaccharide reactive to multivalent ions.

### Claim 15 (depends on 14)

The method according to claim 14, wherein the polysaccharide reactive to multivalent ions is chosen from among an alginate alkaline, a gellan, or a pectin.

### Claim 16 (depends on 5)

The method according to claim 5, wherein that the ion-reactive polyelectrolyte is an alginate alkaline advantageously having an α-L-guluronate block content greater than 55%.

### Claim 17 (depends on 5)

The method according to claim 5, wherein the weight percentage of polyelectrolyte in the second solution (40) is between 0.5 and 3%.

### Claim 18 (depends on 9)

The capsule series (10) according to claim 9, wherein each capsule (10) has a gelled casing (14) with a thickness between 0.1% and 2% of the diameter of the capsule (10).

### Claim 19 (depends on 6)

The method according to claim 6, wherein the weight percentage of polyelectrolyte in the second solution (40) is between 0.5 and 3%.