JP6659075B2 - Capsule body and method for producing the same - Google Patents

Description

  The present invention relates to a capsule body applicable to cosmetics and foods.

In recent years, encapsulation technology has advanced, and small spherical capsules have been used in the fields of cosmetics and foods. This is because the active ingredient and the like can be stably held in the inner phase of the capsule body, and it is suitable for imitation foods such as artificial fish eggs.
Conventionally, capsules of calcium alginate or barium alginate obtained by cross-linking polysaccharide alginic acid with polyvalent ions are often used (Patent Document 1 and the like).
It has been proposed that an arbitrary component can be included in the capsule body during the production process, and that the emulsion or oil component is contained in the internal phase (Patent Document 2 and the like). It has also been proposed to devise an external storage solution of the capsule body in order to retain these internal phase substances and maintain the shape of the capsule body (Patent Document 3).

JP-A-2-117610 JP 2006-174778 A Patent 3151169

Capsules applied to cosmetics and foods are characterized in that they not only retain the internal phase during storage or distribution, but also can be crushed and released during use. For example, in cosmetics, the active ingredient can be arbitrarily released and applied to the skin, and in food, the taste and texture can be enjoyed by chewing like an artificial fish egg.
In a conventional capsule body containing calcium alginate as a main component of the film, the capsule body is easily crushed by reducing the film thickness.

However, when the film thickness is reduced, the capsule body is easily crushed, but the film becomes brittle and it becomes difficult to retain the internal phase, or the internal phase material permeates and releases the membrane when unintended. There is. Further, in the conventional capsule body, there is room for improvement in the feel when the capsule membrane is crushed.
In view of such a situation, the present invention provides a capsule body having a capsule membrane containing calcium alginate, which has a hardness that can be easily crushed and that can suppress permeation and release of an internal phase substance. Make it an issue. It is another object of the present invention to provide a capsule body that can be crushed with a good feel.

  The present inventors have conducted intensive studies in order to solve the above-mentioned problems, and as a result, by adding a water-soluble polymer to the composition of the capsule outer membrane containing calcium alginate, the capsule membrane has a hardness that allows the capsule membrane to be easily crushed while maintaining the internal phase. They have found that permeation and release of substances can be suppressed, and have completed the present invention.

That is, the present invention is as follows.
[1] A capsule body comprising a capsule outer membrane and a capsule inner phase,
The capsule outer membrane includes calcium alginate and a water-soluble polymer,
The capsule internal phase is a capsule body containing an oily component (hereinafter, also referred to as “capsule body of the present invention”).
[2] The capsule according to [1], wherein the water-soluble polymer includes one or more selected from hydroxyethylcellulose, polyvinylpyrrolidone, carboxyvinyl polymer, PEG-based polymer, and acrylic acid-based polymer.
[3] The capsule body according to [1] or [2], wherein the mass ratio between the capsule outer membrane and the capsule inner phase is 2: 8 to 9: 1.
[4] The capsule body according to any one of [1] to [3], wherein the mass ratio of calcium alginate and water-soluble polymer in the capsule outer membrane is 1: 0.1 to 1: 5.
[5] A method for producing a capsule body,
A production method including a step of contacting an aqueous solution containing an alginate and a water-soluble polymer with an aqueous solution containing a calcium salt (hereinafter, also referred to as “the production method of the present invention”).
[6] The method further includes forming a composite droplet by covering the droplet of the solution containing the oily component with a liquid film of an aqueous solution containing an alginate and a water-soluble polymer,
The production method according to [5], wherein a step of contacting an aqueous solution containing an alginate and a water-soluble polymer with an aqueous solution containing a calcium salt is performed by dropping the composite droplet into an aqueous solution containing a calcium salt.
[7] The production according to [5] or [6], wherein the water-soluble polymer includes one or more selected from hydroxyethylcellulose, polyvinylpyrrolidone, carboxyvinyl polymer, PEG-based polymer, and acrylic acid-based polymer. Method.
[8] The method according to any one of [5] to [7], wherein the mass ratio of the alginate and the water-soluble polymer in the aqueous solution containing the alginate and the water-soluble polymer is 1: 0.1 to 1: 5. Production method.
[9] The production method according to any one of [5] to [8], wherein the concentration of the alginate in the aqueous solution containing the alginate and the water-soluble polymer is 0.20 to 2.50% by mass.
[10] The production method according to any one of [5] to [9], wherein the concentration of the water-soluble polymer in the aqueous solution containing the alginate and the water-soluble polymer is 0.1 to 2.0% by mass.
[11] The method according to any one of [5] to [10], wherein the concentration of the calcium salt in the aqueous solution containing the calcium salt is 2.0 to 15% by mass.

ADVANTAGE OF THE INVENTION According to this invention, while having the hardness which is easy to crush, the permeation and discharge | release of an internal phase substance can be suppressed, and also the capsule body with a good feeling at the time of crushing is provided.
Thereby, the feeling of use when the capsule body of the present invention is applied to cosmetics and the texture when applied to foods are excellent.
Further, the capsule of the present invention can suppress permeation of an oily component contained in the internal phase, or can gradually release a scent when a scent releasing component such as a fragrance is contained in the oily component. Therefore, when the capsule body of the present invention is applied to a cosmetic, the quality of the active ingredient can be maintained and the fragrance can be maintained for a long time.

<Capsule of the present invention>
The capsule body of the present invention is a capsule body comprising a capsule outer membrane and a capsule inner phase, wherein the capsule outer membrane contains calcium alginate and a water-soluble polymer, and the capsule inner phase contains an oil component.

The water-soluble polymer in the present specification is not particularly limited as long as it is a polymer that dissolves in distilled water at room temperature at 0.1% by mass or more.
The water-soluble polymer may include two or more kinds of hydroxyethyl cellulose, polyvinylpyrrolidone, carboxyvinyl polymer, PEG-based polymer, acrylic acid-based polymer, or the like in one kind or in an arbitrary combination. Examples of the PEG-based polymer include (PEG-240 / decyltetradeceth-20 / HDI) copolymer, and examples of the acrylic acid-based polymer include (acrylic acid / alkyl acrylate (C10-30)) copolymer and acrylic acid / acrylic. Alkyl / VA) copolymers, alkyl acrylate copolymer ammonium and the like. Of these, hydroxyethylcellulose is particularly preferred because it can provide a more easily crushable hardness.
The water-soluble polymer is not particularly limited, but preferably has a weight average molecular weight of 100,000 to 10,000,000, more preferably 5 to 5,000,000, and further preferably 1 to 2,000,000.

The internal phase of the capsule is usually liquid (at room temperature and under 1 atm). The oil component in the capsule inner phase is not limited to a so-called oil agent, but may be any component that is compatible with petrolatum at room temperature.
As described below, when the capsule body of the present invention is applied to cosmetics, the oily component includes polar oils, natural oils, hydrocarbon oils, silicone oils and the like which are usually used in cosmetics, such as dimethicone and ethyl hexane. Cetyl acid and mineral oil are preferred.
Further, it is preferable to include various oil-soluble active ingredients, for example, a whitening component, an anti-inflammatory component, vitamins, and the like, and an oil-soluble flavor as an oil component in the internal phase. Resorcinols and various plant extracts as whitening ingredients, stearyl glycyrrhetinate and glycyrrhetinyl stearate as anti-inflammatory ingredients, vitamins A and E as vitamins, and hydrocarbon-based fragrances as oil-soluble flavors Aldehyde-based, alcohol-based, phenol-based, acetal-based, ketone-based, ether-based, synthetic musk, lactones, acids, esters, and the like.

In the capsule body of the present invention, the mass ratio of the capsule outer membrane to the capsule inner phase is preferably from 2: 8 to 9: 1, and more preferably from 3: 7 to 6: 4. With such a ratio, the hardness of the capsule body that can be easily crushed can be realized.
In the capsule body of the present invention, the mass ratio of calcium alginate to the water-soluble polymer in the capsule outer membrane is preferably from 1: 0.1 to 1: 5, and preferably from 1: 0.3 to 1: 2. More preferably, the ratio is more preferably 1: 0.4 to 1: 0.9. With such a ratio, the hardness of the capsule body that can be easily crushed can be realized.

The capsule of the present invention is usually spherical. Here, the term “spherical” is not limited to a true spherical shape, and includes a substantially spherical shape, a spheroidal shape, and the like.
The particle size of the capsule body of the present invention is not particularly limited, but is preferably from 0.1 to 50 mm, more preferably from 2 to 8 mm, and still more preferably from 3 to 6 mm.

The capsule body of the present invention can optionally contain other components that can be normally contained in cosmetics and foods.

<Method for producing capsule body of the present invention>
Although not particularly limited, the capsule body of the present invention can be produced by a method including a step of contacting an aqueous solution containing an alginate and a water-soluble polymer with an aqueous solution containing a calcium salt. By such contact, crosslinking of alginic acid by calcium ions starts, and a gel film of calcium alginate is formed. Here, the oily component in the capsule body of the present invention may be included in the capsule membrane of calcium alginate by any method.
A preferred embodiment of the above production method further includes a step of forming a composite droplet by covering a droplet of a solution containing an oily component with a liquid film of an aqueous solution containing alginate and a water-soluble polymer. The step of forming such a composite droplet is performed by, for example, dropping a droplet of a solution containing an oil component inside a droplet of an aqueous solution containing an alginate and a water-soluble polymer, as disclosed in JP-A-5-31787. It can be carried out. In this embodiment, the step of bringing the aqueous solution containing the alginate and the water-soluble polymer into contact with the aqueous solution containing the calcium salt is preferably performed by dropping the composite droplet into the aqueous solution containing the calcium salt. As a result, both solutions are simultaneously dropped into the aqueous solution containing the calcium salt while the aqueous solution containing the alginate and the water-soluble polymer is covered with the solution containing the oily component.

The water-soluble polymer may include two or more kinds of hydroxyethyl cellulose, polyvinylpyrrolidone, carboxyvinyl polymer, PEG-based polymer, acrylic acid-based polymer, or the like in one kind or in an arbitrary combination. Examples of the PEG-based polymer include (PEG-240 / decyltetradeceth-20 / HDI) copolymer, and examples of the acrylic acid-based polymer include (acrylic acid / alkyl acrylate (C10-30)) copolymer and acrylic acid / acrylic. Alkyl / VA) copolymers, alkyl acrylate copolymer ammonium and the like. Of these, hydroxyethylcellulose is particularly preferred because it can provide a more easily crushable hardness.
The water-soluble polymer is not particularly limited, but preferably has a molecular weight of 100,000 to 10,000,000, more preferably 5 to 5,000,000, and further preferably 1 to 2,000,000.

  In an aqueous solution containing an alginate and a water-soluble polymer, the alginate is not particularly limited as long as it is water-soluble. be able to. The weight average molecular weight of the alginate is preferably, for example, 10,000 to 600,000.

The mass ratio between the alginate and the water-soluble polymer in the aqueous solution containing the alginate and the water-soluble polymer is preferably from 1: 0.1 to 1: 5, and preferably from 1: 0.3 to 1: 2. More preferably, it is still more preferably 1: 0.4 to 1: 0.9. With such a ratio, it is possible to manufacture a capsule body having hardness that is easily crushed.
Further, the concentration of alginate in the aqueous solution is preferably 0.20 to 2.50% by mass, more preferably 0.5 to 2.0% by mass, and still more preferably 1.0 to 2.0% by mass.
The concentration of the water-soluble polymer in the aqueous solution is preferably 0.1 to 2.0% by mass, more preferably 0.5 to 1.0% by mass.

In the solution containing the calcium salt, the calcium salt is not particularly limited as long as it is water-soluble, and for example, calcium chloride, calcium sulfate, calcium citrate, calcium phosphate and the like can be used.
Further, the concentration of the calcium salt in the solution is preferably 2.0 to 15% by mass, more preferably 3 to 10% by mass.

In the production method of the present invention, changing the mass ratio between the droplet of the solution containing the oil component and the liquid film of the aqueous solution containing the alginate and the water-soluble polymer to form the above-mentioned composite droplet, and / or By changing the dropping speed of the droplet, the ratio between the internal and external phases and the thickness of the capsule film can be arbitrarily adjusted. Also, by changing the size of the composite droplet, that is, by changing the mass of each solution in the composite droplet, the particle size of the capsule can be arbitrarily adjusted.
Changing the mass of the liquid droplets of the solution containing the oily component or the liquid film of the aqueous solution containing the alginate and the water-soluble polymer can be performed, for example, by changing the nozzle of each nozzle that discharges the solution when forming the liquid droplets or the liquid film of these solutions. This can be achieved by changing the caliber.
The production method of the present invention is performed manually using two syringes, for example, a nozzle that discharges a solution containing an oily component and an aqueous solution containing an alginate and a water-soluble polymer, and the nozzle is discharged from the nozzle. It can be carried out by an apparatus provided with a water tank holding an aqueous solution containing a calcium salt for receiving droplets. An example of such a device is a single-shaft eccentric screw pump.

ADVANTAGE OF THE INVENTION The capsule body of this invention can suppress permeation and discharge | release of an internal phase substance, and has a good feeling at the time of crushing, while having hardness which is easy to crush. Therefore, the components included in the internal phase can be stably maintained, and deterioration can be prevented. Moreover, it can be crushed with an appropriate force and with a good touch. Specifically, it can be crushed without applying excessive force, and it is softly crushed and fits without leaving a feeling of residual or foreign substance on the capsule membrane. In this case, the texture becomes excellent.
Further, since the capsule body of the present invention has a transparent spherical shape, a beautiful appearance can be produced.

The capsule body of the present invention can be preferably applied to cosmetics. For example, a whitening ingredient, an oil-soluble active ingredient such as vitamin A or vitamin E, a fragrance and the like are contained in an internal phase, and a lotion, a cream, a serum, a face wash, It can be blended into hair washes and the like. In particular, when a fragrance is contained in the internal phase, the capsule film does not allow the fragrance to pass too much, so that the fragrance can be released gradually, and the fragrance of the cosmetic can be maintained for a long time.
When the capsule of the present invention is contained in a cosmetic, the aspect is not particularly limited. For example, an aspect in which the cosmetic is constituted by dispersing or immersing the capsule in an aqueous lotion, gel, or the like is preferably mentioned. . In the cosmetic provided in such an embodiment, the capsule membrane is swelled by the aqueous lotion or gel, and the capsule body is more easily crushed. Further, by crushing the capsule body, the oil-soluble component contained in the internal phase can be released in a fresh state into an aqueous lotion or gel phase when the cosmetic is used.

  Further, the capsule body of the present invention can be preferably applied to foods. Calcium alginate has also established its safety as a food.For example, when a cellulosic polymer is used as the water-soluble polymer, it can be applied to imitation foods such as artificial fish eggs and capsules of health foods, etc. In this case, good texture is obtained.

  Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples unless it exceeds the gist.

  According to the formulation of Table 1 below, a capsule body containing an oil component in the internal phase was prepared. Specifically, using a uniaxial eccentric screw pump, the component A filled in the hopper is discharged from the dripping nozzle 1 (diameter 2 mm), and the component B focused on another hopper is discharged from the dripping nozzle 2 (diameter 5 mm). A two-layered composite droplet was formed in which component a was inside and component b was outside. The composite droplet was dropped into component C (calcium chloride solution). In Example 6, the crosslinked capsule body was taken out, washed sufficiently with water, and then added to a water-soluble or oil-soluble gel (d) in an appropriate amount.

<Test Example 1> Sensory evaluation of fragrance release In a 6 cc vial filled with 3 cc of cetyl ethyl hexanoate, 10 capsules of each of the examples or comparative examples washed twice with pure water and cetyl ethyl hexanoate were put. It was allowed to stand at 20 ° C. for 2 weeks. Two weeks later, the fragrance (release) was evaluated at the bottle mouth on the following four scales (n = 3). Table 1 shows the results.
Evaluation conditions;
◎ ・ ・ ・ Not released ○ ・ ・ ・ Almost not released △ ・ ・ ・ Slightly released × ・ ・ ・ Clearly released

<Test Example 2> Quantitative evaluation of fragrance release In Test Example 1, 200 μL of the ethylhexanoic acid solution in which the capsule was immersed for 2 weeks was used as a sample solution. Separately, 0.5 g of the standard reagent was precisely weighed out, and tetrahydrofuran was added to make exactly 50 mL, thereby obtaining a 1% standard stock solution. The standard stock solution was appropriately diluted with tetrahydrofuran to obtain standard solutions of 2000 ppm, 1000 ppm, 500 ppm and 100 ppm.
For each of the sample solution and the standard solution, gas chromatography (GC) / FID analysis was performed under the following conditions, and the limonene concentration was measured by the absolute calibration curve method, and evaluated by the following four steps. Table 1 shows the results.
<< GC measurement conditions >>
Apparatus: Agilent 7890GC
Column: HP-5 0.25 mm ID x 30 m, 0.25 μm
Carrier gas: Helium injection amount: 1 μL
Evaluation conditions;
◎ ・ ・ ・ 0 to 200ppm
○ ・ ・ ・ 200-400ppm
△ ・ ・ ・ 400-800ppm
× ・ ・ ・ 800ppm〜

<Test Example 3> Sensory Evaluation of Easiness of Crushing of Capsule Each capsule body of the example or the comparative example immediately after the preparation was placed on the back of the hand, and the index finger was lightly pressed to give a strain to the side, and the ease of crushing was measured. And the following four grades. Table 1 shows the results.
Evaluation conditions;
◎ ・ ・ ・ Pleasantly crushed ○ ・ ・ ・ Somewhat easy to crush △ ・ ・ ・ Slightly hard but crushed × ・ ・ ・ Hard and not crushable

<Test Example 4> Hardness measurement of capsule body Hardness was measured using a card meter MAX (manufactured by Eye Techno Engineering Co., Ltd.) under the conditions of a pressure-sensitive axis of 11.3 mmφ and a load of 100 g, and evaluated according to the following four grades. Table 1 shows the results.
Evaluation conditions;
◎ ・ ・ ・ 5-15g
○ ・ ・ ・ 15-20g
△ ・ ・ ・ 20-25g
× ・ ・ ・ 30g or more

According to the present invention, the capsule body of the present invention is applied to cosmetics, because the capsule body of the present invention is provided with a capsule body that can suppress the permeation and release of the internal phase substance and has a good feel when crushing while having hardness that is easy to crush. The feeling of use in the case and the texture when applied to food are excellent. Further, when the capsule body of the present invention is applied to cosmetics, the quality of the active ingredient contained in the internal phase can be maintained, and the fragrance can be maintained for a long time.

Claims (7)

A capsule body comprising a capsule outer membrane and a capsule inner phase,
The capsule outer membrane includes calcium alginate and a water-soluble polymer,
The capsule inner phase contains an oily component,
The water-soluble polymer comprises one or more selected from hydroxyethyl cellulose, polyvinylpyrrolidone and acrylic acid-based polymer,
A capsule body, wherein the mass ratio between the capsule outer membrane and the capsule inner phase is 3: 7 to 4: 6 . The capsule body according to claim 1 , wherein the mass ratio between calcium alginate and the water-soluble polymer in the capsule outer membrane is 1: 0.1 to 1: 5. A method for producing a capsule body,
Contacting an aqueous solution containing an alginate and a water-soluble polymer with an aqueous solution containing a calcium salt,
The water-soluble polymer comprises one or more selected from hydroxyethyl cellulose, polyvinylpyrrolidone and acrylic acid-based polymer,
The production method, wherein the mass ratio of the alginate and the water-soluble polymer in the aqueous solution containing the alginate and the water-soluble polymer is 1: 0.3 to 1: 1 . The method further includes forming a composite droplet by covering the droplet of the solution containing the oily component with a liquid film of an aqueous solution containing alginate and a water-soluble polymer,
The production method according to claim 3 , wherein a step of contacting an aqueous solution containing alginate and a water-soluble polymer with an aqueous solution containing a calcium salt is performed by dropping the composite droplet into an aqueous solution containing a calcium salt. The method according to claim 3 , wherein the concentration of the alginate in the aqueous solution containing the alginate and the water-soluble polymer is 0.20 to 2.50 mass%. The method according to any one of claims 3 to 5 , wherein the concentration of the water-soluble polymer in the aqueous solution containing the alginate and the water-soluble polymer is 0.1 to 2.0% by mass. The method according to any one of claims 3 to 6 , wherein the concentration of the calcium salt in the aqueous solution containing the calcium salt is 2.0 to 15% by mass.