JP6682385B2 - Solid composition - Google Patents

Description

  The present invention relates to a solid composition containing a foaming component.

Many solid products using the mechanism that carbon dioxide is generated by the neutralization reaction of carbonate and organic acid are on the market. One of them is an oral solid preparation such as effervescent tablets and effervescent granules, and confectionery such as tablet confections (for example, Patent Documents 1 and 2). These are not only excellent in portability and storability, but when ingested orally, they foam due to contact with saliva and water in the mouth, and rapid disintegration / solubility and unique cooling sensation are gaining popularity. There is.
On the other hand, oral solid preparations that generate carbon dioxide gas in the digestive tract such as the stomach after oral ingestion, such as a gastrointestinal swelling agent for diagnostic imaging of the digestive tract, are not known to cause foaming in the mouth upon oral intake. The gastrointestinal swelling agent is designed to defoam immediately after foaming in the stomach so as not to interfere with contrast enhancement.

  It is known that carbon dioxide gas (air bubbles) accumulates in the stomach for a certain period of time, and when the stomach expands, it stimulates the satiety center of the brain, resulting in abdominal (stomach) bloating and satiety (non- Patent Document 1). Therefore, if it is possible to stably retain the bubbles generated in the stomach after ingestion without erasing the bubbles, it is considered to be useful for, for example, a product which gives a feeling of fullness or a feeling of fullness and controls food intake.

JP-A-2000-239158 JP, 2013-129654, A

J Nutr Sci Vitaminol, 2012, Vol. 58, No. 5, p. 333-338

However, in order to keep air bubbles stable in the stomach, it is necessary to consider that the saliva is almost neutral, while the gastric juice is strongly acidic (pH 1.0-2.0). In addition, in order to allow oral ingestion without difficulty, a flavor suitable for it is required.
Therefore, the present invention relates to providing a solid composition having an excellent durability of foam in the stomach and a good taste.

  As a result of intensive studies to solve the above problems, the present inventors have found that when a foaming component is combined with a predetermined edible surfactant, foaming in the stomach is good, and the resulting foam is gastric for a long time. It was found that it lasts stably. When a foaming component and an edible surfactant are combined, you can feel sourness, bitterness, and astringent taste, but by combining these in a certain range, bitterness and astringent taste are reduced while having a moderate sourness. It was found that a solid composition having a good flavor can be obtained.

That is, the present invention provides the following components (A), (B) and (C):
(A) Edible surfactant having HLB of 12 or more 3 to 60% by mass,
(B) Carbonate 5 to 27% by mass,
(C) Organic acid 5 to 27 mass%
And the neutralization degree of component (C) / component (B) is 1.25 to 7, and the ratio of the total content of component (B) and component (C) to the content of component (A). A solid composition having a (content mass ratio) [{(B) + (C)} / (A)] of 0.6 to 10 is provided.

  According to the present invention, it is possible to provide a solid composition which is excellent in foaming in the stomach and the durability of foam, and which has a suitable sourness but little bitterness and dull taste and has a good flavor.

In the present invention, the “edible surfactant” refers to a surfactant that is generally used for foods and pharmaceuticals. The edible surfactant as the component (A) used in the present invention has an HLB of 12 or more. By containing an edible surfactant having a predetermined HLB in the solid composition together with the foaming component described below, the reaction of the foaming component in the stomach is promoted and the generated foam is stably retained. You can
Here, HLB (hydrophilic-lipophilic balance, Hydrophilic-Lypophilic Balance) indicates the molecular weight of the hydrophilic group portion in the total molecular weight of the surfactant. The HLB of the edible surfactant is calculated by the Griffin equation. When the HLB is composed of two or more kinds of edible surfactants, the HLB value of each edible surfactant is subjected to a phase addition average based on the blending mass ratio.

  (A) The edible surfactant has an HLB of 12 or more, but is preferably 14 or more from the viewpoint of good sustainability of foam in the stomach, and has an HLB of 17 or less. Is preferable, and 16 or less is more preferable.

  Examples of the edible surfactant (A) having an HLB of 12 or more include sucrose fatty acid ester and polyglycerin fatty acid ester.

The sucrose fatty acid ester is a surfactant in which a fatty acid is ester-bonded to the hydroxyl group of sucrose, and may contain a diester, a triester, or a polyester in addition to the monoester.
Among them, the content of the monoester of sucrose fatty acid ester is preferably 60% by mass (hereinafter, referred to as a unit "%") or more, and more preferably 65% or more from the viewpoint of flavor.

  The fatty acid that constitutes the sucrose fatty acid ester is preferably a saturated or unsaturated fatty acid having 12 to 22 carbon atoms, and more preferably a saturated or unsaturated fatty acid having 12 to 18 carbon atoms, from the viewpoint that it can be used in a solid composition. Furthermore, it is preferably a saturated or unsaturated fatty acid having 16 to 18 carbon atoms. Among them, the saturated or unsaturated fatty acid having 18 carbon atoms preferably accounts for 60% or more of the total fatty acid content. As the saturated or unsaturated fatty acid having 18 carbon atoms, stearic acid and oleic acid are preferable, and stearic acid is more preferable.

Polyglycerin fatty acid ester is an ester of polyglycerin and fatty acid. The average degree of polymerization of glycerin in this polyglycerin is preferably 7 or more, and more preferably 10 from the viewpoint that it is widely used and that the foam lasts well. Here, the average degree of polymerization of glycerin refers to a value obtained by an end group analysis method. The terminal group analysis method is the following method. From the relationship between the measured hydroxyl value (OHV) and the theoretical value, the degree of polymerization n and the molecular weight (MW) are calculated by the following equations.
MW = 74n + 18
OHV = 56110 (n + 2) / MW
The hydroxyl value can be measured by acetic anhydride / pyridine method or phthalic anhydride / pyridine method.

  The fatty acid constituting the polyglycerin fatty acid ester is preferably a saturated or unsaturated fatty acid having 12 to 22 carbon atoms, and further a saturated or unsaturated fatty acid having 12 to 18 carbon atoms, from the viewpoint of use in a solid composition. Further, it is preferably a saturated or unsaturated fatty acid having 16 to 18 carbon atoms. Among them, the saturated fatty acid having 18 carbon atoms is preferably 60% or more of the total fatty acid content.

  (A) The edible surfactant having an HLB of 12 or more may be prepared by a known synthesis method, or a commercially available product may be used. If necessary, the commercially available product may be fractionated. , May be prepared by reconstitution.

The edible surfactant (A) having an HLB of 12 or more can be used alone or in combination of two or more.
In the solid composition of the present invention, the content of the edible surfactant (A) HLB of 12 or more is 3 to 60%, but from the point that the sustainability of foam in the stomach is good, It is preferably 5 to 60%, further 5 to 45%, further 10 to 45%, further 10 to 30%.

The solid composition of the present invention contains (B) carbonate and (C) organic acid as foaming components.
Examples of the (B) carbonate used in the present invention include sodium carbonate, sodium hydrogen carbonate, potassium carbonate, potassium hydrogen carbonate, calcium carbonate, magnesium carbonate, sodium sesquicarbonate and the like. Of these, sodium carbonate and sodium hydrogen carbonate are preferable, and sodium hydrogen carbonate is more preferable, from the viewpoints of good foam persistence and good texture.

The carbonate (B) can be used alone or in combination of two or more kinds.
In the solid composition of the present invention, the content of the (B) carbonate is 5 to 27%, but 10 to 25% from the viewpoint that a large amount of foam is generated, bitterness and astringency are reduced. And more preferably 10 to 20%.

  As the organic acid (C) used in the present invention, an edible acid can be used. Examples thereof include organic acids such as citric acid, succinic acid, ascorbic acid, acetic acid, gluconic acid, malic acid, tartaric acid, fumaric acid and adipic acid. Among them, citric acid or malic acid is preferable, and citric acid is more preferable, from the viewpoint that it does not feel an unpleasant taste in the oral cavity and has an appropriate sourness.

The (C) organic acid may be used alone or in combination of two or more kinds.
In the solid composition of the present invention, the content of the organic acid (C) is 5 to 27%, but from the point that a large amount of foam is generated and a suitable sourness is felt, further 10 to 27%, Further, it is preferably 10 to 25%.

  Further, in the solid composition of the present invention, the total content of (B) carbonate and (C) organic acid is from 10 to 54 from the viewpoint that a large amount of bubbles are generated, bitterness and astringency are reduced. %, More preferably 20 to 50%, further preferably 30 to 50%.

In the present invention, the degree of neutralization of component (C) / component (B) is 1.25 to 7.
Here, the degree of neutralization of component (C) / component (B) is a value obtained by dividing the equivalent amount of (C) organic acid contained in the solid composition by the equivalent amount of (B) carbonate. Can be obtained by
Degree of neutralization = {mass% of component (C) / mass% of component (B)} / {component (C) 1 g equivalent / component (B) 1 g equivalent}
From the viewpoint of taste, the degree of neutralization of the component (C) / component (B) is preferably 1.25 to 4, more preferably 1.25 to 3, and further 1.25 to 2. Preferably.

  In the present invention, the total content of (B) carbonate and (C) organic acid in the solid composition is based on the content of the edible surfactant having (A) HLB of 12 or more in the solid composition. The ratio (content ratio by mass) [{(B) + (C)} / (A)] is 0.6 to 10, but the point that the sustainability of bubbles in the stomach is good, bitterness, and ag From the viewpoint of reducing the taste, it is more preferably 0.66 to 6, and further preferably 3 to 6.

  In the solid composition of the present invention, in addition to the above components, in a range that does not impair the effects of the present invention, minerals (for example, calcium, magnesium, iron, zinc, chromium, selenium, manganese, molybdenum, copper, iodine, Phosphorus, potassium, sodium), vitamins (eg vitamin A, vitamin B1, vitamin B2, vitamin B6, vitamin B12, vitamin C, vitamin E, folic acid and salts thereof, or esters thereof), sweeteners (eg fructose) , Monosaccharides such as glucose, galactose, xylose; sucrose, lactose, maltose, trehalose, isomaltooligosaccharides, galactooligosaccharides, fructooligosaccharides, lactose oligosaccharides, soybean oligosaccharides, isomaltulose, coupling sugars and other oligosaccharides ; Sugar alcohol, saccharin, sucralose, stevia, a Sul Pham synthetic sweeteners such as potassium), surfactants other than (A), (C) other than the organic acid acidulant, flavoring, coloring, preservatives, etc. may be appropriately blended.

The solid composition of the present invention generates carbon dioxide gas in the presence of saliva or water in the mouth. In particular, after ingestion, it reacts with water in the stomach to foam, and the resulting foam is stable in the stomach for a long time. Therefore, the solid composition of the present invention is suitable as a product or the like which gives a feeling of fullness and a feeling of fullness in the abdomen (stomach) and controls the intake of food. The pH of gastric juice is generally 1.0 to 2.0, although its acidity changes depending on the situation.
The solid composition of the present invention preferably has a relative foam amount (%) of 45% or more, further 50% or more, further 70 by the foam stability evaluation using a gastric juice model described in Examples described later. % Or more is preferable. It can be judged that the larger this value is, the more excellent the durability of the foam in the stomach is.

  The solid composition of the present invention means a solid composition at room temperature (15 to 25 ° C.), and examples thereof include powder, solid, and granule forms. Further, specific formulations (dosage forms) include, for example, capsules, granules, powders, tablets, pills, troches, and the like. Among them, effervescent tablets, granules, powders, pills, and lozenges are preferable from the viewpoints of easy intake and food, and tablets and granules are preferred because of their short residence time in the oral cavity. Further, a powder is more preferable. The shape of the tablet may be a circular tablet or various irregularly shaped tablets having an oval shape, an oval shape, a square shape or the like. In the case of a circular tablet, a diameter of 5 to 15 mm is preferable from the viewpoint of ingestability. Further, the weight of the tablet is preferably 0.1 to 2 g, more preferably 0.3 to 1 g, per preparation, in terms of simplicity and effectiveness.

  In order to prepare a solid composition, an acceptable carrier can be blended if necessary. For example, excipients (eg starches, crystalline cellulose, light anhydrous silicic acid, calcium hydrogen phosphate, etc.), binders (eg hydroxypropylmethyl cellulose, hydroxypropyl cellulose, gelatin, pregelatinized starch, polyvinylpyrrolidone, polyvinyl alcohol) , Pullulan, methylcellulose, hydrogenated oil, etc.), disintegrant (eg, carmellose, carmellose calcium, croscarmellose sodium, crospovidone, corn starch, low-substituted hydroxypropylcellulose, etc.), lubricant (eg, calcium stearate, Carriers such as magnesium stearate, sodium stearyl fumarate, talc, silicon dioxide), extenders, dispersants, buffers, diluents and the like can be mentioned.

The solid composition of the present invention is not particularly limited and can be produced according to a conventional method.
For example, in the case of producing a powder, (A) an edible surfactant having an HLB of 12 or more, (B) a carbonate, (C) an organic acid, and an additive which is added as necessary are mixed, and the mixture is mixed. The mixture may be used as it is, or the mixture may be crushed before use. The powder preferably passes through the No. 18 (850 μm) sieve in the entire amount, and more preferably remains in the No. 300 (500 μm) sieve at 5% or less of the total amount.

  The granules are prepared by mixing (A) an edible surfactant having an HLB of 12 or more, (B) a carbonate, (C) an organic acid, and an additive added as necessary, and subjecting the mixture to a dry granulation method. It can be obtained by granulating using a wet granulation method or the like. Examples of the granulation method include an extrusion granulation method, a crushing granulation method, a tumbling granulation method, a stirring granulation method, and a fluidized bed granulation method. The average particle size of the granulated product is preferably 45 μm to 850 μm, and more preferably 100 μm to 500 μm.

In the case of producing a tablet, (A) an edible surfactant having an HLB of 12 or more, (B) a carbonate, (C) an organic acid, and an additive added as necessary are mixed, and the mixture is used as a raw material. The powder may be directly compressed and molded, or may be granulated using the dry granulation method, the wet granulation method or the like, and then the granulated product may be compressed by a tablet molding machine to be molded.
When a tablet is produced directly or by compressing a granulated product to form a tablet, a tableting machine such as a rotary tableting machine or a single-shot tableting machine can be used.
The compression molding pressure during tableting is preferably about 10 to 30 MPa from the viewpoint of maintaining the hardness of the molded product.
Further, the tablet hardness is preferably a hardness that can withstand transportation, storage, and the like, and is preferably about 10 N to 200 N in consideration of the sustainability of bubbles in the stomach.

[Carbonate analysis]
The analysis method of the content of carbonate in the solid composition is as follows.
0.1 to 0.2 g of the solid composition was collected, 10 mL of water and 2 mL of 50% phosphoric acid were added, and the container was sealed. After sonication for 10 minutes, one hour left headspace gas determine the amount of CO ₂ was subjected to gas chromatography, was calculated from the generated amount of CO _2.
<Operating conditions for gas chromatograph>
Model: GC-14B [Shimadzu]
Detector: TCD
Column: Chromsorb 101, 80-100 mesh
Glass tube, φ3.2mm × 2m
Temperature: Column 50 ° C, inlet and detector 100 ° C
Cell current 75mA
Gas pressure: Helium (carrier gas) 100 kPa
Injection volume: Headspace gas 0.2mL

[Analysis of organic acids]
The method for analyzing the content of the organic acid in the solid composition is as follows.
1 g of the solid composition was sampled, 20 mL of 5% perchloric acid was added, and the mixture was shaken for 10 minutes for extraction. This was adjusted to 200 mL with water and sonicated for 10 minutes. After filtration, it was subjected to high performance liquid chromatography.
<Operating conditions for high-performance liquid chromatography>
Model: LC-20AD [Shimadzu Corporation]
Detector: UV-visible absorption spectrophotometer SPD-20AV [Shimadzu]
Column: Shim-pack SCR-102H 300 x 80 (length x inner diameter (mm))
[Shimadzu]
Column temperature: 40 ° C
Mobile phase: 3 mm / l perchloric acid reaction solution: 0.2 mm / l containing bromthymol blue 15 mm / l disodium hydrogen phosphate solution flow rate: mobile phase 1.0 mL / min, reaction solution 1.4 mL / min
Measurement wavelength: 445 nm

[material]
SA-1 to SA-19 shown in Table 1 were used as the edible surfactant.

The following raw materials were used.
Sodium hydrogen carbonate: baking soda (Food additive C), Tosoh citric acid: anhydrous citric acid MS, Fuso Chemical Industry Co., Ltd.
Malic acid: Fuso S, Fuso Chemical Industry Co., Ltd.
Succinic acid: succinic acid, Nippon Shokubai Co., Ltd.
Calcium stearate: Aura Bright CA-65, NOF Corporation
Maltitol: Amarti MR-50, Mitsubishi Corporation Foodtech Co., Ltd.

Test Examples 1 to 19
[Preparation of solid composition]
Each raw material component was uniformly mixed in the composition shown in Table 2 to obtain a powdery composition. The numerical value in the parentheses of the edible surfactants (SA-1 to SA-19) indicates HLB. Degree of neutralization of component (C) / component (B) in each composition, of the total content of component (B) and component (C) with respect to the content of edible surfactants (SA-1 to SA-19) The ratio (content mass ratio) was as shown in Table 2.

[Evaluation of foam stability]
The foam stability of the product of the present invention and the comparative product obtained above were evaluated as follows.
(1) Definition and calculation of theoretical foam amount per 1 g The number of moles of carbon dioxide produced by the reaction of the carbonate and the organic acid in the solid composition is obtained by dividing the mass of carbonate by 1 gram equivalent of carbonate. It becomes the smallest value (Mi) of the value and the value obtained by dividing the mass of the organic acid by 1 gram equivalent of the organic acid. On the other hand, the volume of 1 mol of ideal gas is 22.7 liters under standard conditions (0 ° C., 1 bar). Therefore, in the present specification, a value obtained by multiplying Mi by 22.7 liters is defined as a theoretical foam amount (mL) per 1 g of the solid composition.

(2) Gastric fluid model fluid As the gastric fluid model fluid, the disintegration test first fluid (pH 1.2) according to the 16th edition revised Japanese Pharmacopoeia was used.

(3) Definition and calculation of relative foam amount The actual foam amount (measured amount) (mL) generated from 1 g of the solid composition thrown into the gastric juice model liquid is expressed as the theoretical foam amount (mL) per 1 g of the solid composition. The relative foam amount (%) was determined by dividing the value by percentage.
Relative foam amount (%) = [measured amount (mL)] / [theoretical foam amount per 1 g (mL)] × 100
As for the actually measured amount (mL), 1 g of the sample was put into a 50 mL graduated cylinder, 2 mL of the above gastric juice model solution was added, and 0 minutes was set immediately after the addition, and the scale above the foam was read 15 minutes later.
Table 2 shows the theoretical bubble amount (mL), the measured amount (mL), and the relative bubble amount (%) of the product of the present invention and the comparative product.

  As is clear from Table 2, the product of the present invention containing an edible surfactant having an HLB of 12 or more has a higher actual measured amount (mL) and relative foam amount (%) than the comparative product, and therefore, in the stomach. It was confirmed that foaming occurred and that the generated foam remained stable for a long time without disappearing.

Test Examples 20 to 48
[Preparation of solid composition]
Each raw material component was mixed with the composition shown in Table 3 or Table 4 to obtain a powdery composition. The degree of neutralization of component (C) / component (B) in each composition and the ratio of the total content of component (B) and component (C) to the content of component (A) (content mass ratio) are shown in Table 3 or The results are shown in Table 4.

[Evaluation of foam stability]
The foam stability of the inventive product and the comparative product obtained above were evaluated in the same manner. Tables 3 and 4 show the theoretical foam volume (mL), the measured volume (mL) and the relative foam volume (%), respectively.

〔sensory evaluation〕
Further, the invented product and the comparative product were subjected to a sensory evaluation by three expert panels. The evaluation was carried out according to the criteria shown below for the sourness, bitterness and astringency felt when the sample was eaten, and the scores were determined through discussion. The results are shown in Tables 3 and 4.
(Sourness intensity)
5: Weak sourness 4: Slightly sourness 3: Just sourness 2: Slightly sourness 1: Strong sourness (bitterness and astringency)
4: Bitterness and astringency are weak 3: Bitterness and astringency are a little weak 2: Bitterness and astringency are a little strong 1: Bitterness and astringency are strong

As is clear from Tables 3 and 4, it was confirmed that the product of the present invention has a high relative foam amount (%), foams in the stomach, and the foam generated does not disappear and remains stable for a long time. It was In addition, the product of the present invention had a good sourness with little bitterness and astringent taste while having an appropriate sourness.
On the other hand, the comparative product in which the edible surfactant having HLB of 12 or more was not mixed in the predetermined range had a low actual measurement amount (mL) and a relative foam amount (%), and the foam immediately formed in the stomach. It has disappeared. In addition, the strength of sourness was not preferable, and bitterness and astringency were sometimes felt.

Test Examples 49 to 55
[Preparation of solid composition]
Each raw material component was uniformly mixed with the composition shown in Table 5, and then tableted with a ring punch having a hole diameter of 14 mm at a tablet weight of 1000 mg / 1 tablet using a single-shot tableting machine (manufactured by RIKEN). Round tablets were obtained. In Test Examples 49 and 50, Test Examples 51 and 52, and Test Examples 53 and 54, the tableting pressure was adjusted to change the hardness of the tablets. For the tablet hardness, the hardness in the diameter direction was measured using a Hardness Tester (manufactured by Fujiwara Seisakusho).
The degree of neutralization of component (C) / component (B) in each tablet, the ratio of the total content of component (B) and component (C) to the content of component (A) (content mass ratio), tablet hardness, The thickness and diameter are shown in Table 5.

[Evaluation of foam stability]
The foam stability was similarly evaluated for the products of the present invention obtained in Test Examples 49 to 55. Table 5 shows the theoretical foam volume (mL), the actual measurement volume (mL), and the relative foam volume (%).

〔sensory evaluation〕
With respect to the sourness, bitterness and acridness felt when the products of the present invention obtained in Test Examples 49 to 55 were eaten, sensory evaluation was performed by three expert panels in the same manner as above. The results are shown in Table 5.

  As is clear from Table 5, it was confirmed that the product of the present invention has a high relative foam amount (%), foams in the stomach, and the foam generated does not disappear and remains stable for a long time. In contrast to Test Examples 49 and 50, Test Examples 51 and 52, and Test Examples 53 and 54, the one with lower tablet hardness had better foam persistence. In addition, the product of the present invention had a good sourness with little bitterness and astringent taste while having an appropriate sourness.

Claims (5)

The following components (A), (B) and (C):
(A) HLB is 12 or more , and one or more kinds of edible surfactants selected from sucrose fatty acid ester and polyglycerin fatty acid ester 3 to 60% by mass,
(B) Carbonate 5 to 27% by mass,
(C) Organic acid 5 to 27 mass%
And the neutralization degree of component (C) / component (B) is 1.25 to 7, and the ratio of the total content of component (B) and component (C) to the content of component (A). A solid composition in which (content ratio) [{(B) + (C)} / (A)] is 0.6 to 10. Solid composition of claim 1 wherein the fatty acid constituting the sucrose fatty acid esters and polyglycerol fatty acid ester is a saturated fatty acid or unsaturated fatty acids having 12 to 18 carbon atoms. The solid composition according to claim 1 or 2 , wherein the content of the component (A) is 5 to 60% by mass. (C) an organic acid is citric acid, malic acid or solid composition according to any one of claims 1 to 3 which is a combination thereof. Effervescent tablets or foam granule according to claim 1 solid composition according to any one of 4.