JP2000026283A - Powder composition containing oily composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a powder composition resistant to the deterioration and decomposition of an aqueous active component during storage and having the effect for suppressing the taste of the aqueous active component, sustained release effect, masking effect, etc., by dispersing an aqueous active substance in an oil phase in a state of specific fine particles to obtain an oily composition having specific water content or alcoholic aqueous solution content in the solid phase and including the obtained oily composition in the objective composition. SOLUTION: This powder composition contains (A) an oily composition composed of a solid phase containing a water-soluble active substance and/or a water-dispersible active substance and a water-soluble film-forming agent and an oil phase containing an oily component and an emulsifying agent having an HLB of <=10 (e.g. sorbitan monooleate) and (B) a pulverization base. Preferably, the solid phase contains <=30 wt.% of water or an alcoholic aqueous solution and optionally 1-90 wt.% of a polyhydric alcohol and is dispersed in the oil phase in a state of fine particles having an average particle diameter of <=5 μm. The contents of the components A and B in the objective powder composition are preferably 1-80 wt.% and 99-20 wt.%, respectively.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a water-soluble active substance and / or a water-dispersible active substance (hereinafter referred to as an aqueous active substance) which can be used in food, feed, cosmetics, pharmaceuticals, agricultural chemicals, machinery and various other industrial fields. The present invention relates to a powder composition containing an oily composition in which fine particles containing a water-soluble film-forming agent and, in some cases, a polyhydric alcohol or the like are dispersed in an oil phase.

[0002]

BACKGROUND OF THE INVENTION Masking the taste of aqueous active substances,
To have a sustained release function, to increase the absorption in the body,
Aqueous active substances have been encapsulated for the purpose of enhancing long-term storage. Examples of the method for encapsulating the aqueous active ingredient include a core solvation method, a submerged drying method, and a multiple emulsification method. The core solvation method uses a toxic solvent such as formaldehyde or glutaraldehyde as a curing agent. In addition, this preparation method is difficult to commercialize. Japanese Patent Publication No. 7-20859 has been proposed as a capsule of a water-soluble drug using a submerged drying method. However, in general, the in-liquid drying method uses a toxic solvent such as benzene, methylene chloride, chloroform, carbon tetrachloride, and ethyl acetate as the wall film polymer dissolving substance. In the preparation of microcapsules by a submerged drying method, a W / O emulsion containing an aqueous active substance is added to and mixed with an aqueous phase to form a W / O / W emulsion. Since the W / O / W emulsion contains water in the inner aqueous phase, it is inevitable that the aqueous active substance in the inner aqueous phase elutes into the outer aqueous phase. Therefore, in the microcapsules obtained by the submerged drying method, encapsulation of the water-soluble substance was not satisfactory. In Japanese Patent Publication No. 4-24974, etc., W
The W / O / W type emulsified powder is prepared by drying the / O / W type emulsified product, but since the W / O emulsified product is retained even after drying, the inner aqueous phase contains water. I do. Therefore, the internal aqueous phase may rot during long-term storage, the water-soluble substance in the internal aqueous phase may be degraded, or the water of the internal aqueous phase may be eluted into the powder base material and the fluidity of the powder may be reduced. Further, it is difficult to adjust the elution of the water-soluble substance contained in the internal aqueous phase to the outside. Thus, the aqueous active substance-containing capsule obtained by the conventional manufacturing method,
There were various regulations and problems in the materials used, the manufacturing method, the cost, the storage stability, and the like, so that they were not sufficiently satisfactory. In particular, in the fields of foods, medicines, and cosmetics in which raw materials to be used are restricted, it has been difficult to put them to practical use.

[0003]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to suppress the deterioration and decomposition of an aqueous active substance during storage, to reduce the taste of the aqueous active substance, to provide a sustained release effect, a masking effect, and to improve the absorption rate in the body. An object of the present invention is to provide a powder composition having an effect.

[0004]

Means for Solving the Problems In view of the above-mentioned circumstances, the present inventors have made intensive studies and as a result, have found that an aqueous active substance is dispersed in a specific fine particle state in an oil phase, and the water content in a solid phase is reduced. Alternatively, it has been found that a powder composition containing an oily composition having a specific amount of an aqueous alcohol solution can achieve the above object. In the present invention, the solid phase refers to a phase containing an aqueous active substance and a water-soluble film-forming agent, having a water content or an aqueous alcohol content of 30% by weight or less, and optionally containing a polyhydric alcohol or the like. It is. The present invention has been made based on the above findings, and contains an aqueous active substance, a water-soluble film-forming agent, a water content or an aqueous alcohol solution content of 30% by weight or less, and in some cases, a polyhydric alcohol or the like. It is intended to provide a powder composition comprising an oily composition comprising a solid phase to be contained and an oily phase containing an oily component and a lipophilic emulsifier. In the powder composition of the present invention, the oil-based composition particles are adsorbed or included in the powder base material, and the solid phase fine particles are dispersed in the particles. Since the powdery composition of the present invention has a water-based active substance that is not in an aqueous solution state but is coated with an oily component as a solid state like a W / O / W-type emulsifiable powder, deterioration, decomposition, Corrosion and the like can be prevented. Further, unlike the W / O / W type emulsifying powder, the elution of water from the oil phase to the powder base does not occur, so that the powder fluidity does not decrease even after long-term storage. By adjusting the content of the water-soluble film in the solid phase of the powdered oily composition, it becomes possible to adjust the amount of the aqueous active substance eluted into water when the oily composition in the powder comes into contact with water. Furthermore, since the aqueous active substance is coated with the water-soluble film and the oily component in a solid state, when the product of the present invention containing the aqueous active substance absorbed in the intestinal tract is ingested, it binds to the aqueous active substance after ingestion. Less susceptible to gastrointestinal enzymes that digest absorption inhibitors and aqueous active substances. Therefore, the absorption rate is improved because the aqueous active substance is transported to the intestinal absorption site while maintaining the activity.

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the oily composition used in the present invention will be described in detail. The oily composition used in the present invention contains an aqueous active substance and a water-soluble film forming agent,
In some cases, a solid phase containing a polyhydric alcohol or the like,
An oil component and an oil phase containing an emulsifier having an HLB of 10 or less.

First, the solid phase of the oily composition used in the present invention will be described. The aqueous active substance used in the present invention may be any substance that dissolves in water and / or disperses in water, but is preferably one that dissolves in water or an aqueous alcohol solution. In addition, there is no limitation on the method for producing the aqueous active substance. For example, acidulants, pigments, colorants, flavors, antioxidants, enzymes, fungi, seasonings, inorganic salts, starch,
Starch hydrolyzate, peptide, biologically active polypeptide, amino acid, dietary fiber, cellulose, nutritional enhancer,
Herbal extract, antidiabetic, antipyretic, anti-inflammatory, analgesic,
Sedatives, antiallergic agents, antibiotics, antiulcer agents, antitumor agents, anticoagulants, hemostatic agents, cardiotonic agents, muscle relaxants, anesthetics, arrhythmic drugs, vasodilators, etc., vaccines, animal and plant extracts Substances, specifically, citric acid and its salts, phosphoric acid and its salts, metaphosphoric acid and its salts, gardenia blue pigment, caramel, cacao pigment, grape skin pigment, strawberry pigment, perilla pigment, phospholipase , Amylase, dehydrogenase, takapiastase N1, lactic acid bacteria, butyric acid bacteria, bifidobacteria, nucleic acids, yeast, taurine, salt, soy sauce, sodium carbonate, sodium citrate, corn starch, dextrin, milk peptide, corn peptide, insulin, somatostatin, thyroid stimulation Hormones, parathyroid hormone, growth hormone, luteinizing hormone-releasing hormone, - tryptophan, lysine chloride, sodium glutamate, sodium aspartate, polydextrose, microcrystalline cellulose, ascorbic acid and salts thereof, nicotinamide, nicotinic acid,
Phosphate L-magnesium ascorbate, vitamin B
, Niacin, calcium pantothenate, folic acid, biotin, calcium salts such as calcium chloride, milk mineral, calcium lactate, casein calcium peptide (CCP), casein phosphopeptide (CPP), calcium cytoremate (CCM), Beef bone meal, shell powder, heme iron, zinc, arbutin, kojic acid, nifedipine, ubidecarenone, nicardipine, methotrexate, somatostatin, fenformin hydrochloride, glipizide, buformin hydrochloride, glymidine sodium, sodium salicylate, sodium flufenamic acid, sulpirin, Prochlorperazine, chlorpromazine hydrochloride, diphenhydramine hydrochloride, methdilazine hydrochloride, chlorpheniramine maleate, amikacin, tobramycin, ribidomycin, gentamicin , Canendomycin, tetracycline hydrochloride, dibekacin, ampicillin, metoclopromide, mitomycin C, bleomycin hydrochloride, actinomycin D, methotrexate, daunorubicin hydrochloride, vincristine sulfate, bisblastine sulfate, adriamycin, lentinan, glycyrrhizin, heparin sodium, thrombin, thromboplastin Pioxocamphor, aminophylline, theophyllol, pridinol methanesulfonate, tubocurarine chloride, bufetrol hydrochloride, diltiazem hydrochloride, oxyphedone hydrochloride, dipotassium glycyrrhizinate, clophenylamine maleate, codeine phosphate, aspirin, acetaminophenone, d-maleic acid Chlorpheniramine, tipepidine hibenzate, visbentia , Magnesium aluminate metasilicate, carbetapentane citrate, potassium guaiacolsulfonate, influenza vaccine, gymnema, gymnemasylvesta extract, barley extract, honey, royal jelly, propolis, arhat extract, herbal extract, grape extract, blueberry Extract, Blueberry leaf extract, Rosemary extract, Tea extract, Catechin, Tochu extract, Roth extract, Pollen, Naringin, Spice extract, Kokemo extract, Caffeine, Oubak powder, Iodine, Cobalt, Selenium ,
Oligosaccharides, xylooligosaccharides, garlic extract, shiitake mushroom extract, wasabi, ash, Matsuba extract, basil, coca,
Sansho, shiso, shiso extract, hot pepper, rice bran enzyme digest, chlorella, taurine, spirulina, eleuthero, chitin, chitosan, rutin, safflower extract, green coffee bean extract, sunflower seed extract, aloe, isoalpha bitterness Acid, gentian extract, reishi, reishi extract, cordyceps, mamushi extract, mallow extract, turtle extract, oyster extract, mugwort extract, kukushi, wolfberry, kumazasa extract, ginseng extract, ginseng extract, ginkgo leaf extract, Ginseng leaf extract, octacosanol, peonies,
Engosaku, Ryokyo, Shukusha, Borei, Engosaku, Keihi Extract, Daidai Extract, Oyster Leaf Extract, Kuzu Flower Extract, Fennel Extract, Ginger Extract, Eleuthero, Hawthorn Extract, Guarana Extract, Oyster Extract, Licorice Extract, Isoleucine,
Threonine, phenylalanine, naringin, niacinamide, lysine, threonine, arginine, guarana,
Examples include oyster extract, gymnema sylvestre extract, reindeer horn extract, stevia, deep-sea shark extract, fur seal extract, shirako protein, and placenta extract. The aqueous active substance may be used alone or 2
A combination of more than two types may be used. The content of the aqueous active substance is 5 to 95% by weight, preferably 5 to 80% by weight based on the total weight of the solid phase of the oily composition.
And more preferably 10 to 70% by weight.

The water-soluble film-forming agent used in the present invention forms a film when the aqueous solution is dried. Examples thereof include gelatin, glue, gum arabic, starch microbial culture, hemicellulose, and water-soluble film-forming agent. And synthetic polymers. The above-mentioned gelatin refers to a polypeptide obtained by treating collagen such as degraded, extracted, purified, and dried in a large amount in bones and skins of animals, and is used in fields such as food, feed, cosmetics, pharmaceuticals, and industry. Can be used without particular limitation. Further, purified gelatin which has been subjected to bleaching purification can also be used. The glue described above is a gelatin containing a large amount of impurities and generally used in the fields of food, feed, cosmetics, pharmaceuticals, industry and the like. The above gum arabic is
It is commonly used in the fields of food, feed, cosmetics, pharmaceuticals, industry and the like. The above-mentioned starch microbial culture is a neutral polysaccharide obtained by subjecting starch to microbial cultivation and then subjecting it to extraction, purification, drying, and the like, and is generally used in the fields of food, feed, cosmetics, pharmaceuticals, industry, and the like. is there. Examples of the starch microorganism culture include pullulan. The hemicellulose is a water-soluble polysaccharide extracted and purified from conifers, hardwoods, grasses, seeds, seed coats, and the like,
Further, these are subjected to a chemical treatment with an acid, an alkali or the like,
It has been hydrolyzed by physical treatment with heat, pressure, or the like, or biological treatment with an enzyme or the like. The above-mentioned hemicellulose is generally used in the fields of food, feed, cosmetics, pharmaceuticals, industry and the like. As hemicellulose,
For example, arabinogalactan extracted and purified from larch trees, corn fiber extracted and purified from maize seed coat (for example, Cell Ace # 40 manufactured by Nippon Shokuhin Kako Co., Ltd.), and fiber extracted and purified from soybean (non- Soya Five-S, manufactured by Nii Oil Co., Ltd., and xylan of flour. The water-soluble film-forming synthetic polymer used in the present invention includes, for example, carboxymethylcellulose, methylcellulose, cellulose acetate phthalate, sodium polyacrylate, polyvinyl alcohol, polyvinylpyrrolidone, polyvinylmethylether, carboxyvinyl polymer, hydroxyethylcellulose, hydroxypropyl Methyl cellulose, carbopol, and poly (methyl vinyl ether / maleic anhydride), which are generally used in the fields of cosmetics, pharmaceuticals, industry, and the like. The water-soluble film forming agents may be used alone or in combination of two or more. The content of the water-soluble film-forming agent in the solid phase is 1 to 95% by weight, preferably 5 to 80% by weight, more preferably 10 to 70% by weight. Since the solidification of the water-soluble film covering the aqueous active ingredient prevents the solid phases from coalescing, the dispersion stability of the solid phase in the oil phase is improved. When the water-soluble film forming agent is not blended, the storage stability of the dispersed oil is reduced. Further, by adjusting the amount of the water-soluble film-forming agent added, it becomes possible to adjust the amount of the aqueous active substance eluted into water when the oily composition comes into contact with water. That is, the aqueous active substance 1
When the amount of the water-soluble film-forming agent is less than 50 parts by weight, preferably less than 25 parts by weight, the aqueous active substance gradually elutes from the oily composition to external water. When the amount of the water-soluble film-forming agent is more than 50 parts by weight, preferably 80 parts by weight, more preferably more than 100 parts by weight, the elution of the aqueous active substance from the oily composition to the external water per 100 parts by weight Can be considerably reduced.

Various polyhydric alcohols can be used in the present invention, and water-soluble alcohols having 2 or more, more preferably 2 to 12, and more preferably 2 to 6 hydroxyl groups in the molecule can be used. Is good. For example, glucose, maltose, maltitol, sorbitan, sorbitol, sucrose, lactose, fructose, xylitol, inositol, erythritol, pentaerythritol, propylene glycol, 1,3-butylene glycol, ethylene glycol, glycerin, diglycerin, triglycerin, poly Glycerin (average degree of polymerization: 4 to 10), saccharified reduced starch, fructose fructose liquid sugar, fructose dextrose liquid sugar, and the like can be given. These can be used alone or in combination of two or more. By adding the polyhydric alcohol to the solid phase, the long-term storage at 40 ° C. and the freezing resistance of the oily composition are further improved. The content of the polyhydric alcohol in the solid phase is 1 to 90% by weight, preferably 5 to 8%.
0% by weight, more preferably 5 to 70% by weight. Here, in the solid phase, both a water-soluble film forming agent and a polyhydric alcohol may be contained, or only the water-soluble film forming agent or only a polyhydric alcohol may be contained.

[0009] If necessary, a thickening stabilizer can be added to the solid phase of the oily composition used in the present invention. Xanthan gum, guar gum, locust bean gum, carrageenan, agar,
Pectin, sodium alginate, gellan gum and the like. When a thickener is added, its content is preferably 0.01 to 5% by weight in the solid phase of the oily composition.

[0010] The water used in the present invention is not particularly limited, and purified water, distilled water, tap water and the like can be used. In addition, alcohol can be added to the water.
Examples of the alcohol include monohydric alcohols such as ethanol and methanol. In this case, the amount of the alcohol used is 1 to 300 parts per 100 parts by weight of water.
It is preferably about parts by weight.

[0011] If necessary, an emulsifier having an HLB of 10 or more can be added to the solid phase of the oily composition used in the present invention. The emulsifier used preferably has an HLB of 20 or less. Emulsifiers having an HLB of 10 or more include sucrose fatty acid ester, polyglycerin fatty acid ester, extracted lecithin, enzymatically decomposed lecithin, hydrogenated lecithin, saponin, glycolipid, protein, protein hydrolyzate (excluding gelatin and glue), silicone System emulsifier, alkylene oxide addition emulsifier, and the like. HLB is 10
When the above emulsifier is added, its content is preferably 0.01 to 5% by weight based on the total weight of the oil composition.

Further, known additives such as preservatives, coloring agents, perfumes, and pH adjusters can be added to the solid phase of the oily composition used in the present invention. When the additive is added, its content is preferably 0.01 to 5% by weight based on the total weight of the solid phase of the oily composition.

The solid phase of the oily composition used in the present invention has a water content or an aqueous alcohol solution content of 30.
% By weight or less, preferably 20% by weight or less,
It is more preferably at most 10% by weight, most preferably at most 5% by weight. When the water content or the aqueous alcohol solution content in the solid phase is more than 30% by weight, the storage stability of the oily composition is reduced, and the aqueous active substance is deteriorated. When a powder composition is prepared using this oily composition, it is difficult to stably disperse the aqueous active substance in the oil phase particles. The method for reducing the water content or the aqueous alcohol solution content of the solid phase of the oily composition used in the present invention to 30% by weight or less is not particularly limited. Examples thereof include vacuum drying, heat drying, thin film distillation drying, and freeze drying. It can be carried out by the method described above.

The solid phase of the oily composition used in the present invention is dispersed in the oil phase described below in the form of fine particles having an average particle diameter of 5 μm or less. The average particle size of the solid phase is preferably 3 μm or less, more preferably 0.05 to 2 μm.
It is. When the average particle size of the solid phase is larger than 5 μm, the storage stability of the oily composition is significantly reduced. When a powder composition is prepared using this oily composition, it is difficult to stably disperse the solid phase fine particles in the oil phase particles. There is no particular limitation on the method of converting the solid phase dispersed in the oil phase into fine particles having an average particle diameter of 5 μm or less. For example, while slowly mixing the oil phase and the aqueous phase, about 30
Minutes, emulsified or high pressure homogenizer,
Finally, using an emulsifier such as a microfluidizer,
/ O type emulsion is obtained and dried. Here, “to finally obtain a W / O emulsion”
Even if it is W / O type or O / W type at the initial stage of emulsification,
Even if it is a mixture of a mold and a W / O type, it means that it is sufficient that the mixture finally becomes a W / O type. In the present invention, the average particle diameter of the solid phase is a value measured by using a laser diffraction type particle size distribution analyzer (LA-500, manufactured by Horiba, Ltd.).

Next, the oil phase of the oil composition used in the present invention will be described. The oil phase contains an emulsifier and an oil component. Foods, as the emulsifier,
Known emulsifiers used in the fields of feed, cosmetics, pharmaceuticals, industry and the like can be used without particular limitation except as described below. As the emulsifier used in the present invention, it is preferable to use an emulsifier having an HLB of 10 or less.
It is preferable to use an emulsifier having an HLB of 1 or more. H
When only an emulsifier having an LB greater than 10 is used, W / O
An oily composition cannot be obtained because a type emulsion cannot be prepared.

Examples of the emulsifier having an HLB of 10 or less include sorbitan fatty acid ester, glycerin fatty acid ester, organic acid monoglyceride, propylene glycol fatty acid ester, diglyceride, sucrose fatty acid ester, polyglycerin fatty acid ester, hydrogenated lecithin, lecithin, silicone And a surfactant such as a sorbitan monooleate, a sorbitan distearate, a polyoxyethylene (6 mol) sorbitan monostearate, a glycerin monostearate, a glycerin monolinolate, and a citric acid. Esterification of acid and glycerin monooleate, propylene glycol monostearate, glycerindiolate, glycerin dilinoleate, and transesterification of rapeseed oil and glycerin. Diglyceride obtained, diglyceride obtained by transesterification of safflower and glycerin, diglycerin distearate, diglycerin tristearate, hexaglycerin triolate, hexaglycerin pentastearate, tetraglycerin condensed ricinoleate, polyglycerin condensed ricinolein Acid ester, sucrose tri-pentastearate, polyoxyethylene (5 mol) cetyl ether, polyoxyethylene (3 mol) nonylphenyl ether,
Polyoxyethylene (6 mol) stearyl ether, polyoxyethylene (5 mol) hydrogenated castor oil, polyoxyethylene (15 mol) hydrogenated castor oil, polyoxyethylene (20 mol) sorbitol tetraolate, lecithin (Nisshin Oil Co., Ltd. ), Lecithin DX, Basis LP-2
0), hydrogenated lecithin (Basis LP, manufactured by Nisshin Oil Co., Ltd.)
-20H), dimethylsiloxane / methyl (addition of 5 moles of polyoxyethylene) siloxane copolymer, dimethylsiloxane / methyl (addition of 5 moles of polyoxyethylene), siloxane / methyl (addition of 5 moles of polyoxypropylene)
Examples include siloxane copolymers. In the present invention, the above-mentioned emulsifiers may be used alone or in combination of two or more.

In the present invention, an emulsifier having an HLB of 10 or more may be used in combination with an emulsifier having an HLB of 10 or less. Examples of such emulsifiers include sucrose fatty acid esters, polyglycerin fatty acid esters, extracted lecithin, enzymatically decomposed lecithin, hydrogenated lecithin, saponins, glycolipids, proteins, protein hydrolysates (excluding gelatin and glue), silicones Surfactants and alkylene oxide-added surfactants. Specifically, sucrose stearic acid monoester, hexaglycerin oleic acid monoester, decaglycerin stearic acid monoester, extracted lecithin (manufactured by Nisshin Oil Co., Ltd., Basis LS-6)
0), enzymatically-decomposed lecithin (Basis LG-10K, Basis LP-20E, manufactured by Nisshin Oil Co., Ltd.), hydrogenated lecithin (Basis LS-60H, manufactured by Nisshin Oil Co., Ltd.), Kiyala saponin, soybean protein hydrolysate Degradation products, sodium caseinate,
Wheat gluten hydrolyzate, dimethylsiloxane / methyl (polyoxyethylene 60 mol addition) siloxane copolymer, polyoxyethylene (25 mol) hydrogenated castor oil, polyoxyethylene (80 mol) hydrogenated castor oil, and the like. In the present invention, it is particularly desirable to use polyglycerin condensed ricinoleate alone or in combination with polyglycerin fatty acid ester, glycerin monofatty acid ester or lecithin. In the present invention, one or a combination of two or more of the above emulsifiers can be used in combination with a lipophilic emulsifier.

As the oil component used in the present invention, known oil components used in the fields of food, feed, cosmetics, pharmaceuticals, industry and the like can be used without particular limitation. The oily component is in a liquid state, but may be in a liquid state at normal temperature, or may be used without particular limitation as long as it can be dissolved by heating. Examples of the oily component include enzymatic treatment of hydrocarbons, esters, animal and vegetable fats and oils, waxes, goby fat, higher fatty acids, higher alcohols, silicone-based substances, sterols, and resins. (Hydrolysis, transesterification, etc.) and chemically treated (transesterification, hydrogenation, etc.), etc. From the viewpoint of production and handling, it is preferable to use an oil phase which is liquid or fluid at normal temperature. Examples of these are soybean oil, rapeseed oil, corn oil,
Sesame oil, cottonseed oil, safflower oil, sunflower oil, peanut oil, rice germ oil, wheat germ oil, brown rice germ oil, oat oil,
Macadamian nut oil, garlic oil, camellia oil,
Palm oil, olive oil, jojoba oil, macadamian nut oil, avocado oil, castor oil, linseed oil, perilla oil, eucalyptus oil, evening primrose oil, turtle oil, mink oil, lard, tallow,
Horse oil, snake oil, fish oil, egg oil, egg yolk oil, liquid paraffin, isoparaffin, petrolatum, squalane, squalene, turpentine oil, isopropyl myristate, isopalmityl myristate, 2-octyldodecyl myristate, 2- Cetyl ethylhexanoate, glyceryl tri-2-ethylhexanoate, glyceryl tri-caprylate, triglyceride of mixed fatty acid of caprylic acid and capric acid, di-2
-Neopentyl glycol ethylhexanoate,
Diisostearyl malate, isononyl isononanoate (3,5,5-trimethylhexyl-
3 ', 5', 5'-trimethylhexanoate), 12
Cholesteryl hydroxystearate, monoester or hexaester of isostearic acid and / or higher fatty acid and dipentaerythritol manufactured by Emery Co., glycerol ester of paramethoxycinnamic acid and 2-ethylhexanoic acid, iso-paramethoxycinnamate Octyl ester and the like can be mentioned.

Hardened soybean oil, hardened rapeseed oil, hardened palm oil, hardened fish oil, glyceryl tristearate, rosin, cholesterol, phytosterols (campesterol, stigmasterol, sitosterol, etc.), orange roughy oil, lanolin, Myristic acid,
Palmitic acid, isopalmitic acid, stearic acid, isomeric isoleic acid, linoleic acid,
Linolenic acid, ricinoleic acid, 12-hydroxystearic acid, 10-hydroxystearic acid, behenic acid, erucic acid, arachidonic acid, eicosapentaenoic acid, docosahexaenoic acid, myristyl alcohol, cetyl alcohol, stearyl alcohol, isostearyl alcohol, behenyl alcohol, lanolin Alcohol, paraffin wax, microcrystalline wax, ceresin wax, beeswax, petrolatum, hard fat, carnauba wax, candelilla wax, rice wax, rice bran wax, wood wax shellac, dimethyl polysiloxane, methylphenyl polysiloxane, essential oils derived from animals and plants Components and the like can also be targeted. These oil components may be used alone or in combination of two or more. The content of the emulsifier in the oil phase of the oily composition used in the present invention is preferably 0.5 to 50.
%, More preferably 1 to 30% by weight.

The oil phase of the oily composition used in the present invention may contain known additives such as preservatives, coloring agents and fragrances. When the additive is added, the amount of the additive is preferably 0.01 to 5% by weight based on the total weight of the oil phase of the oily composition. In the oily composition used in the present invention, the oil phase may contain an oil-soluble active substance. The oil-soluble active substance, for example, antioxidants,
Nutrient enhancers, drugs and animal and plant extracts; specifically, mixed tocopherol, dl-α-tocopherol, acetate-dl-α-tocopherol, tocotrienol, EPA, DHA, sesame oil extract, β -Carotene, vitamin A, rosemary oil, vitamin Ds, vitamin Ks, essential fatty acids, rice bran oil extract, γ-oryzanol, assembly extract, propolis extract, sage extract, pepper extract, squalene, terrapin oil, Liver oil and the like. The oil-soluble active substances may be used alone or in combination of two or more. When the oil-soluble active substance is contained in the oil phase, its content is preferably 0.1 to 99% based on the total weight of the oil phase.
%, More preferably 0.2 to 40% by weight.

The oily composition used in the present invention contains the solid phase in an amount of 5 to 75% by weight, preferably 10 to 60% by weight,
It is preferable that the oil phase contains 95 to 25% by weight, preferably 90 to 40% by weight.

The method for producing the oily composition used in the present invention is not particularly limited. For example, it can be produced by the method described below. The method for producing the oily composition used in the present invention is an aqueous active substance, a water-soluble film forming agent,
Adjusting the aqueous phase containing water to 10-90 ° C.,
Mixing the oily component and an oil phase containing an emulsifier into a final W / O emulsion, and then subjecting the solid phase to a drying treatment so that the water content or the aqueous alcohol solution content is 30% by weight or less. Consists of When a polyhydric alcohol, a thickening stabilizer, a monohydric alcohol, or the like is added, the polyhydric alcohol is mixed and dissolved in the aqueous phase. The above-mentioned aqueous active substance, water-soluble film-forming agent, polyhydric alcohol, thickening stabilizer, water, monohydric alcohol, oily component and emulsifier are the same as those contained in the oily composition used in the present invention. Is used. In the method for producing an oily composition used in the present invention, first, an aqueous active substance and a water-soluble film forming agent are mixed with water to form an aqueous phase. In the aqueous phase, a water-soluble film forming agent,
When adding a polyhydric alcohol, a thickening stabilizer, a monohydric alcohol, or the like, they are mixed with the aqueous phase here. In addition, an additive or the like that can be contained in the solid phase of the oily composition used in the present invention may be added to the aqueous phase. Next, the aqueous phase is adjusted to a temperature of 10 to 90C. Further, an emulsifier and an oil component are mixed to form an oil phase. The mixing ratio of the emulsifier in the oil phase is preferably from 0.5 to 50% by weight, more preferably from 1 to 30% by weight, based on the total weight of the oil phase. Further, an oily effective substance, an additive, and the like that can be contained in the oil phase of the oil composition used in the present invention may be added to the oil phase. Next, the oil phase and the aqueous phase are mixed to finally form a W / O emulsion. In this case, it is preferable to adjust the oil phase to a temperature of 10 to 90 ° C. By heating the oil phase, it becomes possible to add an oil component in a solid state at normal temperature. The mixing ratio of the aqueous phase and the oil phase (parts by weight of the aqueous phase / parts by weight of the oil phase) is preferably 95/5 to 1/95.
99, more preferably 85/15 to 20/80.
It is.

The mixture of the water phase and the oil phase is finally mixed with W /
As a method for preparing an O-type emulsion, a conventionally known method can be used without any particular limitation. For example, a mixture of the above-mentioned water phase and oil phase is treated with a propeller, a homomixer, a homodisper, a high-pressure homogenizer, a microfluidizer. And the like, emulsification using an emulsifier. Then, the W / O emulsion is subjected to a drying treatment so that the water content or the aqueous alcohol solution content in the solid phase is 30% by weight or less, preferably 0 to 20% by weight, more preferably 0 to 10% by weight. %, Most preferably from 0 to 5% by weight, to give an oily composition. When the W / O emulsion in which the lipophilic emulsifier is densely arranged around the aqueous phase is dried to form a solid phase, the solid phase is formed in a state where the hydrophilic portion of the lipophilic emulsifier is incorporated in the solid phase. , It is considered that the dispersion stability of the solid phase in oil becomes very high. The method for drying the W / O emulsion is not particularly limited, and examples thereof include methods such as vacuum drying, heat drying, thin film distillation drying, and freeze drying.
Moreover, you may carry out in the state which warmed the said W / O type emulsion, and may perform after cooling the said W / O type emulsion to refrigeration temperature-room temperature.

Next, the powder composition of the present invention will be described in detail. The powder composition of the present invention comprises the above oily composition containing an aqueous effective substance and a powdered base material, and optionally an emulsifier, and is obtained by adsorbing or including the oily composition on the powdered base material. . The powder composition of the present invention contains the oily composition described above in an amount of 1 to 80% by weight, preferably 5 to 60% by weight, more preferably 10 to 50% by weight. % By weight, preferably 95 to 40% by weight, more preferably 90 to 50% by weight.

The powdered base material of the powdered composition of the present invention is a substance capable of adsorbing or encapsulating oil, such as starch, starch hydrolyzate, cyclodextrin, protein, protein hydrolyzate, complex protein, and processed protein. Examples include starch, polyhydric alcohol, gum arabic, thickening stabilizer, starch microbial culture, hemicellulose, water-soluble film-forming synthetic polymer, and the like. The powdered base material may be used alone, or two or more kinds may be used in combination. The starch, starch hydrolyzate, cyclodextrin, protein, protein hydrolyzate, and composite protein used as the powdered base are, for example, corn starch, potato starch, wheat starch, rice starch, tapioca starch, or a mixture of these starches. Hydrolyzate, α-cyclodextrin, corn protein, soy protein, sodium caseinate, glycoprotein, skim milk, and hydrolyzate of these proteins, gelatin,
Glue, wheat gluten hydrolyzate, lecithin protein complex and the like. The processed starch used for the powdered base material is obtained by processing starch or starch hydrolyzate, for example, oxidized starch, monostarch phosphate, distarch phosphate, phosphorylated distarch phosphate, Acetylated starch diester, acetylated starch, acetylated distarch adipic acid, hydroxypropyl distarch phosphate, sodium octenylsuccinate starch, sodium octenylsuccinate starch hydrolyzate, and the like. As the polyhydric alcohol used for the powdered base material, the same polyhydric alcohol that can be used for the above-described oily composition can be used. Thickening stabilizers used in the powdered base material include, for example, xanthan gum, guar gum, locust bean gum, carrageenan, agar, pectin,
Sodium alginate, gellan gum and the like.
The same starch microbial culture that can be used in the oily composition described above can be used as the starch microbial culture used for the powdered substrate. The same hemicellulose that can be used for the above-described oily composition can be used as the hemicellulose used for the powdered base material. As the water-soluble film-forming synthetic polymer used for the powdered base material, the same water-soluble film-forming synthetic polymer that can be used for the oil-based composition described above can be used. The above powdered base materials may be used alone or in combination of two or more. The content of the powdered base material is 2% based on the total weight of the powdery composition.
It is from 0 to 99% by weight, preferably from 40 to 95% by weight, more preferably from 50 to 90% by weight.

Further, by blending an emulsifier with the powder composition, a powder composition having better fluidity and water dispersibility can be obtained. The emulsifier is an emulsifier having an HLB of 10 or less and an HLB which can be used for the oily composition described above.
The same thing as ten or more emulsifiers can be used. The emulsifiers may be used alone or in combination of two or more. A preferred amount of the emulsifier is
0.01 to 15% by weight based on the total weight of the powdery composition,
Preferably it is 0.01 to 10% by weight.

The powder composition of the present invention may further contain a known powder fluidity improver (such as calcium lactate or silica gel),
Coloring agents, fragrances, pH adjusters and the like can be blended or added. When the additive is added, the amount of the additive is preferably 0.01 to 5% by weight based on the weight of the powder.
It is.

The method for producing the emulsified composition of the present invention is not particularly limited. For example, it can be produced by the method described below. After dissolving or dispersing the powdered base material in water, adding the oily composition containing an aqueous active substance,
Using an emulsifier such as a propeller, a homomixer, a homodisper, a high-pressure homogenizer, and a microfluidizer, an emulsion is prepared in which the oily composition is used as an internal phase and the powdered base material solution is used as an external phase. The temperature at the time of emulsification is preferably adjusted to 10 to 90 ° C. The powder composition of the present invention is obtained by evaporating water from the emulsion using a method such as drying under reduced pressure, drying by heating, drying by thin-film distillation, and freeze-drying.
Here, when an emulsifier having an HLB of 10 or less is added, the emulsifier is preferably added to the oily composition.
When 0 or more emulsifiers are added, they are preferably added to water. Mixing ratio of the oily composition and the powdered substrate (parts by weight of the oily composition / parts by weight of the powdered substrate)
Is 1/99 to 80/20, preferably 5/9
5/60/40, more preferably 10/90 ~
50/50. Further, as a simple production method, a powder adsorption method described below can be mentioned. After the powdered base material is charged into a stirrer such as a Hobart mixer or a Henschel mixer, the oily composition is slowly charged and mixed into the flowing powdered base material to thereby mix the powdered composition of the present invention. obtain.

[0029] The powder composition of the present invention can be prepared by diluting water or / and a monohydric alcohol,
It can be used for feed, cosmetics, industrial products, pharmaceuticals and the like. The powder composition of the present invention includes noodles such as ramen, tanmen, udon, buckwheat, macaroni, spaghetti, fried noodles, non-fried noodles, powders and liquid soups, sauces, yogurt, prepared milk, infant milk powder, ice cream, yogurt,
Dairy products such as cream and whipped cream, rice crackers, snacks, biscuits, wafers, chocolate, candy,
Caramel, gum, candy, gummy and other confectionery, chikuwa, kamaboko, fish meat sausage, fish meat ham and other fishery products, frozen tempura, frozen deep-fried, frozen fried, frozen dumplings, frozen dumplings and other frozen foods, miso, hamburger,
Ham, sausage, gyoza, shumai, bread, cooking oil,
Butter, margarine, shortening, cheese, mayonnaise, dressing, beverages, health foods, foods such as therapeutic foods, lipsticks, cosmetic creams, emulsions, shampoos, rinses, packs, cataplasms, etc., nutrition drinks,
It can be used for pharmaceuticals such as powders, tablets, ointments and vitamins and quasi-drugs, industrial products such as fertilizers and lubricating oils, and other feeds.

When the powder composition of the present invention is poured into water, an aqueous solution in which oil particles containing fine particles of an aqueous active substance are dispersed is obtained. Further, by adjusting the amount of the water-soluble film-forming agent of the solid phase dispersed in the oily composition in the powder composition, the amount of the aqueous active substance dissolved in water when the oily composition comes into contact with water can be adjusted. It becomes possible. In other words, when the amount of the water-soluble film-forming agent is less than 50 parts by weight, preferably less than 25 parts by weight, based on 100 parts by weight of the aqueous active substance, the aqueous active substance is discharged from the oily composition to the outside. It is gradually eluted (sustained release effect), but the amount of the water-soluble film forming agent is 5 per 100 parts by weight of the aqueous active substance.
When the amount is more than 0 parts by weight, preferably 80 parts by weight, more preferably more than 100 parts by weight, the dissolution of the aqueous active substance from the oily composition to the outside can be considerably suppressed (elution suppressing effect). The powder composition of the present invention containing the aqueous active substance having umami, sweetness or aroma, which has a sustained release effect by the above method, gradually releases the umami, sweetness or aroma to the outside, and has a Has a lasting effect. In addition, the powder composition of the present invention containing an aqueous active substance having bitterness and astringency, which has an elution suppressing effect by the above method, hardly feels its taste, so that it can be used in the foods and pharmaceuticals. I feel little bitterness. The powder composition of the present invention can be used as a health food or medicine in the form of tablets or granules. The powder composition of the present invention can be used in the form of being encapsulated in known capsules (eg, gelatin capsules and agar capsules). Conventionally, aqueous active substances and oily active substances have been separately added to foods, feeds, cosmetics, industrial products, and pharmaceuticals.However, in the emulsified composition and powder composition of the present invention, aqueous active substances And the oily active substance can be added at the same time.
In addition, since the aqueous effective substance is coated with the oily component in a solid state instead of an aqueous state, deterioration, decomposition, decay, etc. of the aqueous effective substance itself can be prevented. further,
Since the aqueous active substance is coated with the water-soluble film and the oily component in a solid state, when the product of the present invention containing the aqueous active substance that is absorbed in the intestinal tract is ingested, absorption inhibition that binds to the aqueous active substance after ingestion is suppressed. Less susceptible to gastrointestinal enzymes that digest substances and aqueous active substances. Therefore, the absorption rate is improved because the aqueous active substance is transported to the intestinal absorption site while maintaining the activity.

[0031]

(Aqueous active substance content in solid phase)

Content of aqueous active substance in solid phase (% by weight) = (weight of aqueous active substance / (weight of water or alcohol aqueous solution in oily composition + weight of solid phase excluding water or alcohol aqueous solution)) ×
100 [Water-soluble film-forming agent content in solid phase] Water-soluble film-forming agent content in solid phase (% by weight) =
(Water-soluble film-forming agent weight / (Water or alcohol aqueous solution in oily composition + Solid phase weight excluding water or alcohol aqueous solution)) × 100 [Polyhydric alcohol content in solid phase] Polyhydric alcohol content (% by weight) = (weight of polyhydric alcohol (solid content) / (weight of water or alcohol aqueous solution in oily composition + weight of solid phase excluding water or alcohol aqueous solution)) × 100 [average of solid phase] Particle diameter] The average particle diameter of the solid phase of the oily composition is measured by a laser diffraction particle size distribution analyzer (LA-500).
Mold, manufactured by Horiba, Ltd.).

Reference Example 1 Reishi extract powder 70.0 g, gelatin (manufactured by Miyagi Chemical Industry Co., Ltd., gelatin AU) 30.0 g, water 520.0
g and heated to 60 ° C. to obtain an aqueous phase, 350.0 g of soybean oil, tetraglycerin tristearate (manufactured by Sakamoto Pharmaceutical Co., Ltd., SY Glister TS-310, H
LB: 4) 30.0 g was mixed and dissolved at 60 ° C. to obtain an oil phase. While slowly adding the aqueous phase to the oil phase, using a homomixer at 6000 rpm for 20 minutes,
A W / O emulsion was obtained by mixing and emulsifying at 60 ° C.
Next, the obtained emulsion was dehydrated under reduced pressure using an oil pump to obtain a liquid brown oily composition containing 14.5% by weight of Reishi extract. The water content in the oily composition was 0.5% by weight. The water content in the solid phase dispersed in the oil phase is 2.3% by weight, the content of Ganoderma extract is 68.4% by weight, and the amount of gelatin relative to 100 parts by weight of Ganoderma extract is 42.9. Parts by weight. The gelatin content in the solid phase was 29.3% by weight. The average particle size of the solid phase was 1.2 μm. The storage stability of the obtained oily composition was evaluated by the following method. Table 1 shows the evaluation results.

[Storage stability of oily composition] The obtained oily composition was placed in a thermostat at 5 ° C and 40 ° C for 1 month and 3 months.
The appearance of the oil composition after storage for 1 month and 6 months was visually observed. The appearance of the oily composition after storing the oily composition at room temperature for 1 month, 3 months, and 6 months was also visually observed. Each was evaluated according to the following evaluation criteria. The table also shows the visual observations immediately after production. A: No abnormality was observed in the oily composition. ：: Oil phase separation of less than 1% of the total volume was observed. Δ: Oil phase separation of 1 to 5% of the total volume was observed. ：: Oil phase separation of 5% or more of the total volume was observed. □: Solid phase (or aqueous phase) separation of less than 1% of the total volume was observed. (2): Solid phase (or aqueous phase) separation of 1% or more of the total volume was observed. X: Mold occurred.

Reference Example 2 Reishi extract powder 70.0 g, Gelatin AU, 120.0 g
g, 430.0 g of water and heated to 60 ° C. to form an aqueous phase, 350.0 g of soybean oil, SY Glister TS-
An oil phase was obtained by mixing 310 and 30.0 g and dissolving at 60 ° C. In the same manner as in Reference Example 1, a liquid brown oily composition containing 12.3% by weight of Reishi extract was obtained. The water content in the oily composition was 0% by weight.
The water content in the solid phase dispersed in the oil phase was 0% by weight, the content of Ganoderma extract was 36.8% by weight, and the amount of gelatin was 171.4 parts by weight based on 100 parts by weight of Ganoderma extract. Met. The gelatin content in the solid phase was 63.
It was 2% by weight. The average particle size of the solid phase was 0.9 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Reference Example 3 Reishi extract powder 70.0 g, gelatin AU, 120.0 g
g, D-sorbitol solution (manufactured by Towa Chemical Industry Co., Ltd., sorbit L-70, water content: 30% by weight) 70.0
g, water (360.0 g) and heated to 60 ° C. to form an aqueous phase, soybean oil (350.0 g), SY Glister TS-
An oil phase was obtained by mixing 310 and 30.0 g and dissolving at 60 ° C. In the same manner as in Reference Example 1, a liquid brown oily composition containing 11.2% by weight of Reishi extract was obtained. The water content in the oily composition was 0.6% by weight. The water content in the solid phase dispersed in the oil phase is 1.
5 wt%, the content of Ganoderma extract was 28.8% by weight, and the amount of gelatin per 100 parts by weight of Ganoderma extract was 171.
It was 4 parts by weight. The gelatin content in the solid phase was 49.4% by weight, and the D-sorbitol content was 20.2% by weight. The average particle size of the solid phase was 0.6 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Reference Example 4 80.0 g of sodium glutamate, water-soluble soybean fiber (Soyafive-S, manufactured by Fuji Oil Co., Ltd.) 16.0
g, water (454.0 g) and heated to 60 ° C. to form an aqueous phase, soybean oil (395.0 g), soybean hardened oil (Nissin Oil Co., Ltd., soybean hardened oil (34 °), 5.0 g), Polyglycerin condensed ricinoleate (RIKEN Vitamin Co., Ltd.)
Manufactured by Poem PR-300, HLB: 1.7) 45.0 g
And 5.0 g of glycerin fatty acid monoester (Emulgy MU, HLB: 4.2, manufactured by Riken Vitamin Co., Ltd.)
Were dissolved at 60 ° C. to obtain an oil phase. Thereafter, sodium glutamate 1 was prepared in the same manner as in Reference Example 1.
A liquid white oily composition containing 4.2% by weight was obtained. The water content in the oily composition was 3.4% by weight. The water content in the solid phase dispersed in the oil phase is 16.6% by weight, and the content of sodium glutamate is 69.5% by weight.
The amount of the water-soluble soybean fiber was 100 parts by weight based on 100 parts by weight of sodium glutamate. The water-soluble soy fiber content in the solid phase was 13.9% by weight.
Met. The average particle size of the solid phase was 0.5 μm.
The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Reference Example 5 Tea extract (Sanphenon, manufactured by Taiyo Kagaku Co., Ltd.) 90.0
g and pullulan (Pulllan manufactured by Hayashibara Co., Ltd.) 80.0 g,
A mixture of 1.0 g of guar gum (manufactured by Saneigen FFI Co., Ltd., Bistop B-20) and 399.0 g of water 6
What was heated to 0 ° C. was used as an aqueous phase, soybean oil 400.0 g,
Hexaglycerin pentaolate (Sakamoto Pharmaceutical Co., Ltd.)
Manufactured by SY Glister PO-500, HLB: 4) 30.
An oil phase was obtained by mixing and dissolving 0 g at 60 ° C.
Thereafter, a liquid brown oily composition containing 14.9% by weight of a tea extract was obtained in the same manner as in Reference Example 1. The water content in the oily composition was 0.3% by weight. The water content in the solid phase dispersed in the oil phase was 1.0% by weight, the content of the tea extract was 52.1% by weight, and the amount of pullulan per 100 parts by weight of the tea extract was 88.9. Parts by weight. The pullulan content in the solid phase was 46.3% by weight. The average particle size of the solid phase was 0.4 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Reference Example 6 70.0 g of ascorbic acid, gelatin AU, 70.0 g
g, water-soluble corn fiber (Nippon Shokuhin Kako Co., Ltd.)
Cell Ace # 25) 30.0 g, enzyme-degraded lecithin (Nisshin Oil Co., Ltd., Basis LG-10K) 1.0 g, water 4
An aqueous phase (60 ° C.) was obtained by mixing and dissolving 29.0 g,
Medium chain fatty acid triglyceride (OD, manufactured by Nisshin Oil Co., Ltd.)
O) 300.0 g, tocopherol (Nissin Oil Co., Ltd.)
Manufactured by Tocopherol 100), 50.0 g, Poem PR-
300 and 50.0 g were mixed and dissolved at 60 ° C. to obtain an oil phase. Thereafter, a liquid white oily composition containing 12.2% by weight of ascorbic acid was obtained in the same manner as in Reference Example 1. The water content in the oily composition was 0.3% by weight. The water content in the solid phase dispersed in the oil phase is 1.0% by weight, the ascorbic acid content is 40.5% by weight, and the amount of gelatin and corn fiber relative to 100 parts by weight of ascorbic acid is 142.9. Parts by weight. The content of gelatin and corn fiber in the solid phase was 57.9% by weight. The average particle size of the solid phase is 0.8
μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Reference Example 7 50.0 g of calcium chloride, gelatin AU, 100.
0 g, 30.0 g of reduced starch saccharified solution (Amamiru, water content: 30% by weight, manufactured by Towa Chemical Industry Co., Ltd.), water 46
The aqueous phase was obtained by mixing 0.0 g and heating to 60 ° C.
250.0 g of soybean oil, refined fish oil (manufactured by Tama Seikagaku Co., Ltd.
DHA-27) 50.0 g, SY Glister TS-31
An oil phase was prepared by mixing 0, 10.0 g and 50.0 g of glycerindiolate and dissolving at 60 ° C. Thereafter, a liquid white oily composition containing 9.8% by weight of calcium chloride was obtained in the same manner as in Reference Example 1. The water content in the oily composition was 2.8% by weight. The water content in the solid phase dispersed in the oil phase is 9.6% by weight, the content of calcium chloride is 33.2% by weight,
The amount of gelatin relative to 0 parts by weight was 130 parts by weight. The gelatin content in the solid phase was 43.2% by weight, and the reduced starch saccharified substance content was 14.0% by weight.
The average particle size of the solid phase was 0.7 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

REFERENCE EXAMPLE 8 Ginseng extract 80.0 g, gelatin (manufactured by Nitta Gelatin Co., Ltd., gelatin MJ) 55.0 g, Sorbit L-
70, 50.0 g, 10% by weight aqueous ethanol solution 51
The aqueous phase (60 ° C.) obtained by mixing and dissolving 7.0 g was soy oil 250.0 g, wood wax 3.0 g, Poem PR-30.
0, 40.0 g, citrate monoglyceride (manufactured by Riken Vitamin Co., Ltd., Poem K-30, HLB: 3) 5.0 g
Were dissolved at 60 ° C. to obtain an oil phase. A liquid brown oily composition containing 17.1% by weight of ginseng extract was obtained in the same manner as in Reference Example 1. The water content in the oily composition was 0.2% by weight. The water content in the solid phase dispersed in the oil phase was 0.6% by weight, the content of ginseng extract was 46.8% by weight, and the amount of gelatin relative to 100 parts by weight of ginseng extract was 68.8 parts by weight. there were. The gelatin content in the solid phase was 32.2% by weight, and the D-sorbitol content was 20.5% by weight.
The average particle size of the solid phase was 1.2 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

[0041] Reference Example 9 vitamin B ₁ 40.0g and Arabic gum (Sanei chemical Trade Co., Ltd., Arabic call SS) 60.0g, glycerin 200.0g, a mixture of water 370.0g 60 ℃ to warming The water phase is used as the aqueous phase, ODO, 300.0 g, SY
Glister PO-500, 30.0 g, mixed at 60 ° C
The oily phase was used as the oil phase. Thereafter, a liquid translucent yellow oily composition containing 6.3% by weight of vitamin B ₁ was obtained in the same manner as in Reference Example 1. The water content in the oily composition was 0.1% by weight. The water content of the solid phase dispersed in the oil phase is 0.2 wt%, the content of vitamin B ₁ represents 13.3% by weight, the amount of gum arabic to vitamin B ₁ 100 parts by weight 150 parts by weight Department. The gum arabic content in the solid phase is 20.0% by weight,
The glycerin content was 66.5% by weight. The average particle size of the solid phase was 0.3 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Reference Example 10 Vitamin B ₁ 20.0 g, Arabic Cole SS, 4
0.0 g of polyoxyethylene tetraoleate (40
Mol) sorbit (manufactured by Kao Corporation, Leodor 440)
HLB: 11.8) 1.0 g, glycerin 20.0 g,
An aqueous phase (60 ° C.) obtained by mixing and dissolving 504.0 g of water was used as an aqueous phase (60 ° C.), 300.0 g of glyceryl tri-2-ethylhexanoate (TIO, manufactured by Nisshin Oil Co., Ltd.), and liquid paraffin 5
0.0 g, squalane 5.0 g, hexaglycerin condensed ricinoleate (manufactured by Sakamoto Pharmaceutical Co., Ltd., SY
55.0 g of Glyster CR-500, HLB: 2), hydrogenated lecithin (manufactured by Nisshin Oil Co., Ltd., Basis LP-20)
H) 5.0 g was mixed and dissolved at 60 ° C. to obtain an oil phase. While slowly adding the aqueous phase to the oil phase, the mixture was emulsified at 6000 rpm for 20 minutes at 60 ° C. using a homomixer, and then 100 kg / cm 2 using a high-pressure homogenizer.
By emulsifying at a pressure of ^2, a W / O emulsion was obtained. Then, to obtain an oily liquid composition yellow containing vitamin B ₁ 4.0 wt% by the emulsion obtained are dehydrated under reduced pressure using an oil pump. The water content in the oily composition was 0.2% by weight. The water content in the solid phase dispersed in the oil phase is 1.2% by weight, and vitamin B ₁
The content of 24.4 wt%, the amount of gum arabic to vitamin B ₁ 100 parts by weight was 200 parts by weight. The gum arabic content in the solid phase was 48.8% by weight,
The glycerin content was 24.4% by weight. The average particle size of the solid phase was 0.2 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Reference Example 11 0.4 g of insulin, 4.0 g of gelatin A-U, 2.0 g of glycerin, and 60.6 g of 0.1N hydrochloric acid aqueous solution were mixed at 30 ° C. to obtain an aqueous phase. 0.0 g,
30 g of SY Glister TS-310 mixed with 3.0 g
What was melt | dissolved at C was made into the oil phase. While slowly adding the aqueous phase to the oil phase, use a homomixer to mix
By mixing and emulsifying at 30 ° C. for 10 minutes at rpm, W /
An O emulsion was obtained. Next, the obtained emulsion was dehydrated under reduced pressure at 30 ° C. using an oil pump to obtain a liquid white oily composition containing 1.0% by weight of insulin.
The water content in the oily composition was 0.1% by weight. The water content in the solid phase dispersed in the oil phase was 0.6% by weight, the insulin content was 6.2% by weight, and the amount of gelatin relative to 100 parts by weight of insulin was 1000 parts by weight. The gelatin content in the solid phase was 62.1% by weight, and the glycerin content was 31.1% by weight. The average particle size of the solid phase was 1.8 μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 1 shows the evaluation results.

Comparative Reference Example 1 Reishi extract powder 70.0 g, gelatin AU, 120.0 g
g, sorbit L-70, 70.0 g, water 360.0 g
And heated to 60 ° C. to form an aqueous phase, soybean oil 3
50.0 g, SY Glister TS-310, 30.0 g
Were dissolved at 60 ° C. to obtain an oil phase. The water phase was slowly added to the oil phase, and the mixture was emulsified with a stirring bar for 20 minutes to obtain a W / O emulsion. Next, the obtained emulsion was dehydrated under reduced pressure using an oil pump to obtain a liquid brown oily composition containing 11.3% by weight of Reishi extract. The water content in the oily composition is 0.2
% By weight. The water content in the solid phase dispersed in the oil phase is 0.5% by weight, and the content of Reishi extract is 29.1.
In terms of% by weight, the amount of gelatin per 100 parts by weight of Reishi extract was 171.4 parts by weight. The gelatin content in the solid phase was 50.0% by weight, and the D-sorbitol content was 20.4% by weight. The average particle size of the solid phase is 7.2
μm. The storage stability of the obtained oily composition was evaluated in the same manner as in Reference Example 1. Table 2 shows the evaluation results.

Comparative Reference Example 2 Reishi extract powder 70.0 g, gelatin AU, 120.0 g
g, sorbit L-70, 70.0 g, water 360.0 g
And heated to 60 ° C. to form an aqueous phase, soybean oil 3
50.0 g, SY Glister TS-310, 30.0 g
Were dissolved at 60 ° C. to obtain an oil phase. A liquid brown W / O emulsion containing 7.0% by weight of Reishi extract was obtained by mixing and emulsifying at 60 ° C. for 20 minutes at 6000 rpm using a homomixer while slowly adding the aqueous phase to the oil phase. Was. The water content in the emulsion is 38.1
% By weight. The water content in the aqueous phase was 61.5% by weight, the content of Reishi extract was 11.3% by weight, and the amount of gelatin relative to 100 parts by weight of Reishi extract was 171.4 parts by weight. The gelatin content in the aqueous phase was 19.3.
% By weight, the D-sorbite content was 7.9% by weight, and the average particle size of the emulsified particles was 1.8 μm. The same evaluation as in Reference Example 1 was performed for the storage stability of the obtained emulsion composition. Table 2 shows the evaluation results.

Comparative Reference Example 3 70.0 g of ascorbic acid, gelatin AU, 70.0 g
g, Cell Ace # 25, 30.0 g, Basis LG-1
A solution obtained by mixing and dissolving 1.0 g of 0K and 429.0 g of water was used as an aqueous phase (60 ° C.), and ODO, 300.0 g, tocopherol 100, 50.0 g, Poem PR-300,
A mixture obtained by mixing 0.0 g and dissolving at 60 ° C. was used as an oil phase. A W / O emulsion was obtained by mixing and emulsifying at 60 ° C. for 20 minutes at 6000 rpm using a homomixer while slowly adding the aqueous phase to the oil phase. Next, the obtained emulsion was dried using an oil pump for a shorter time than in Reference Example 6, so that liquid white W containing 10.7% by weight of ascorbic acid and having a higher moisture content than Reference Example 6. / O emulsion was obtained. The water content in the emulsion is 12.
7% by weight. The water content in the aqueous phase was 32.6% by weight, the content of ascorbic acid was 27.6% by weight, and the amount of gelatin and corn fiber relative to 100 parts by weight of ascorbic acid was 142.9 parts by weight. The content of gelatin and corn fiber in the aqueous phase was 39.4% by weight. The average particle size of the emulsified particles was 1.4 μm. The same evaluation as in Reference Example 1 was performed for the storage stability of the obtained emulsion composition. Table 2 shows the evaluation results.

Comparative Reference Example 4 Reishi extract powder 70.0 g, gelatin AU, 120.0 g
g, sorbit L-70, 70.0 g, water 360.0
g, decaglycerin monooleate (Sakamoto Pharmaceutical Co., Ltd.)
SY Glister MO-750, HLB: 13) 3
The aqueous phase was obtained by mixing 0.0 g and heating to 60 ° C.
What melt | dissolved 350.0 g of soybean oil at 60 degreeC was used as the oil phase. While the aqueous phase was slowly added to the oil phase, mixed emulsification was performed at 6000 rpm for 20 minutes at 60 ° C. using a homomixer, but the W / O emulsion was phase-inverted to become an O / W emulsion. As a result, no oily composition was obtained.

[0048]

[Table 1]

[0049]

[Table 2]

Example 1 30 g of the oily composition obtained in Reference Example 1, glycerin fatty acid monoester (Emulgy MU, manufactured by Riken Vitamin Co., Ltd.)
0.5 g were mixed and heated to 60 ° C. 20 g of chemically modified starch (Emulstar # 30A, manufactured by Matsutani Chemical Industry Co., Ltd.), 149.5 g of starch hydrolyzate (Paindex # 3, manufactured by Matsutani Chemical Industry Co., Ltd.) and 400 g of water were mixed and heated to 60 ° C. This was used as the aqueous phase. 4000 rp using a homomixer while slowly adding the oily composition to the aqueous phase.
By emulsifying at 20 m for 20 minutes, a white emulsion was obtained. By spray-drying this emulsion,
A powder composition having good fluidity containing the Reishi extract was obtained.
In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 2 30 g of the oily composition obtained in Reference Example 2 and Emulgy MU0.
5 g were mixed and heated to 60 ° C. Emulstar # 30
A, 20 g, par index # 3, 149.5 g, water 4
The resulting mixture was heated to 60 ° C., and the resulting mixture was used as an aqueous phase.
Thereafter, the same operation as in Example 1 was performed to obtain a powder composition having good fluidity containing the Reishi extract. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 3 30 g of the oily composition obtained in Reference Example 3, Emulgy MU0.
5 g were mixed and heated to 60 ° C. Emulstar # 30
A, 20 g, par index # 3, 149.5 g, water 4
The resulting mixture was heated to 60 ° C., and the resulting mixture was used as an aqueous phase.
Thereafter, the same operation as in Example 1 was performed to obtain a powder composition having good fluidity containing the Reishi extract. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 4 30 g of the oily composition obtained in Reference Example 4, Emulgy MU0.
5 g were mixed and heated to 60 ° C. Emulstar # 30
A, 20 g, par index # 3, 149.5 g, water 4
The resulting mixture was heated to 60 ° C., and the resulting mixture was used as an aqueous phase.
Thereafter, the same operation as in Example 1 was performed to obtain a powder composition having good fluidity containing sodium glutamate. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 5 20 g of the oily composition obtained in Reference Example 5 was used as an oil phase (60 ° C.). Hexaglycerol monooleate (Sakamoto Yakuhin Kogyo Co., Ltd., SY Glister MO-500) 1 g, pullulan (Hayashibara Co., Ltd., pullulan) 5 g, Paindex #
3, 174 g and 400 g of water were mixed and heated to 60 ° C. to obtain an aqueous phase. While slowly adding the oil phase to the aqueous phase, the mixture was emulsified at 6000 rpm for 20 minutes using a homomixer, and then 50 kg / cm using a high-pressure homogenizer.
By emulsifying at a pressure of ² , a yellow emulsion was obtained. By spray-drying this emulsion,
A powder composition containing tea extract and having good fluidity was obtained. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 6 160 g of a starch hydrolyzate (Paindex # 1 manufactured by Matsutani Chemical Industry Co., Ltd.) was charged into a Hobart mixer, and the oily composition obtained in Reference Example 6 was added while the powder was being rotated and fluidized. After slowly dropping 40 g (50 ° C.) of the product, the mixture was stirred for 20 minutes to obtain a powder composition containing ascorbic acid and having good fluidity. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 7 80 g of the oily composition obtained in Reference Example 7 was heated to 60 ° C.
Soy protein hydrolyzate (Solpy 20 manufactured by Nisshin Oil Co., Ltd.)
00) 4 g, par index # 3, 116 g, water 400
g and heated to 60 ° C. to form an aqueous phase. Thereafter, the same operation as in Example 1 was performed to obtain a white emulsion. This emulsion was freeze-dried to obtain a powder composition having good flowability containing calcium chloride. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 8 40 g of the oily composition obtained in Reference Example 8 was heated to 60 ° C.
Gum arabic (Arabic Cole SS, manufactured by Sanei Pharmaceutical Trading Co., Ltd.) 60 g, Paindex # 3, 100 g, water 4
The resulting mixture was heated to 60 ° C., and the resulting mixture was used as an aqueous phase.
The oily composition was slowly added to the aqueous phase and emulsified at 6000 rpm for 20 minutes using a homomixer to obtain a brown emulsion. The emulsion was freeze-dried to obtain a powder composition containing ginseng extract with good fluidity. In addition, 1 g of the obtained powder composition
Was added to 99 g of water to obtain a white emulsion. When this emulsion was observed with a microscope, it was found that 5
Solid phase fine particles of μm or less were present.

Example 9 160 g of parindex was put into a Hobart mixer,
The powder to where that rotates flow, after slowly added dropwise to the oily composition obtained in Reference Example 9 40g (50 ℃), by stirring for 20 minutes, the fluidity good powder composition containing vitamin B ₁ Obtained. In addition, 1 g of the obtained powder composition
Was added to 99 g of water to obtain a white emulsion. When this emulsion was observed with a microscope, it was found that 5
Solid phase fine particles of μm or less were present.

Example 10 160 g of Paindex # 1 was charged into a Hobart mixer, and the powder was rotated and fluidized.
After slowly dropping 40 g (50 ° C.) of the oily composition obtained in the above,
By stirring for 20 minutes to obtain a flowable good powder composition containing vitamin B _1. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Example 11 190 g of parindex # 1 was charged into a Hobart mixer, and the powder was rotated and fluidized.
After slowly dropping 10 g (30 ° C.) of the oily composition obtained in the above,
By stirring for 20 minutes, a powder composition having good fluidity containing insulin was obtained. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. When this emulsion was observed with a microscope, solid phase fine particles of 5 μm or less were present in the oil particles.

Comparative Example 1 30 g of the W / O emulsion obtained in Comparative Reference Example 1 and 0.5 g of Emulgy MU were mixed and heated to 60 ° C. Emulstar # 30A, 20g, Paindex # 3, 149.5
g and 400 g of water and heated to 60 ° C. to obtain an aqueous phase. Thereafter, the same operation as in Example 1 was carried out to obtain a powder composition having good fluidity containing the Reishi extract. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. The emulsion was observed with a microscope, but no particles were present in the oil particles.

Comparative Example 2 30 g of the oily composition obtained in Comparative Reference Example 2, Emulgy MU
0.5 g was mixed and heated to 60 ° C. Emulstar # 3
A mixture of 0A, 20 g, Paindex # 3, 149.5 g, and 400 g of water and heated to 60 ° C. was used as an aqueous phase. Thereafter, the same operation as in Example 1 was performed to obtain a powder composition containing the reishi extract. The resulting powder composition had many small lumps and was moist and had poor powder properties. Also, 1 g of the obtained powder composition was added to water 99
By adding to g, a white emulsion was obtained. The emulsion was observed with a microscope, but no particles were present in the oil particles.

Comparative Example 3 40 g of the oily composition obtained in Comparative Reference Example 3 (50 ° C.) was slowly dropped into 160 g of Paindex # 1 in a Hobart mixer while the powder was being rotated and fluidized. By stirring for minutes, a powder composition containing ascorbic acid was obtained. The resulting powder composition was a moist, low-flow powder. In addition, a white emulsion was obtained by adding 1 g of the obtained powder composition to 99 g of water. The emulsion was observed with a microscope, but no particles were present in the oil particles.

(Taste Test of Powder Composition Containing a Specific Oily Composition) The taste test of the powder compositions containing various aqueous active substances prepared in Examples 1 to 10 and Comparative Examples 1 to 3 was carried out on a healthy person 20. Conducted on the first name. 30 g of the powder composition
Was also mixed immediately after mixing with 100 g of water and after stirring the propeller for 3 hours. Table 3 shows the results.

[0065]

[Table 3]

[Storage Stability Test of Aqueous Active Substance] The residual ratio (%) of ascorbic acid when the powder compositions of Example 6 and Comparative Example 3 were stored in a thermostat at 40 ° C. for one month was examined. The measurement of the residual ratio of ascorbic acid was performed using a high performance liquid chromatography method. Table 4 shows the results.

[0067]

[Table 4]

[Calcium Absorption Test] Calcium chloride powder or the powder composition of Example 7 was mixed with feed so that the calcium content was 0.2%, and each feed was mixed with a Wistar male rat 10 having a body weight of about 200 g. The animals were fed for 10 days, and a calcium balance experiment was performed to determine the calcium absorption rate. Table 5 shows the results of the calcium absorption test.
Shown in

[0069]

[Table 5]

[Insulin Absorbency Test] An insulin solution prepared with a physiological saline phosphate solution or the powder composition of Example 11 was used to give 50 U / kg of insulin to 10 Wistar male rats weighing about 200 g. Was orally administered for 5 days, blood was collected on the last day of the administration, and the blood glucose level in the blood was examined. As a result, the blood glucose level of the rats to which the insulin solution was orally administered was almost unchanged as compared to before the insulin administration, but the blood glucose level of the rats to which the powder composition of Example 11 was orally administered was decreased. .

[0071]

As described in detail above, the powder composition of the present invention is obtained by adsorbing and enclosing a specific oily composition in a powder base material. Specific oily compositions are aqueous active substances,
A solid phase containing a water-soluble film-forming agent, preferably containing a polyhydric alcohol;
An oily composition comprising an oil phase containing 0 or less emulsifier, wherein the solid phase is dispersed in the oil phase in a fine particle state having an average particle diameter of 5 μm or less, and The water content is 30% by weight or less. for that reason,
In the powder composition containing the specific oily composition, the taste of the aqueous active substance is reduced or masked, and the aqueous active substance is hardly deteriorated. In addition, the rate of absorption of the aqueous active substance in the body can be improved. Further, the powder composition of the present invention has a taste-reducing effect, a sustained-release effect, a masking effect, and an effect of improving the absorption rate in the body of the aqueous active substance, and thus can be used in foods, feeds, pharmaceuticals, and agricultural chemicals. Further, since the water-based active substance hardly deteriorates, it can be used in machines and other various industrial fields.

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Claims (8)

[Claims] 1. A solid phase containing a water-soluble active substance and / or a water-dispersible active substance and a water-soluble film forming agent, and an oil phase containing an oil component and an emulsifier having an HLB of 10 or less. Wherein the solid phase is dispersed in the oil phase in the form of fine particles having an average particle diameter of 5 μm or less, and the water content or the aqueous alcohol content of the solid phase is 30% by weight or less. The oily composition is
A powder composition comprising a powdered base material. 2. A powder composition comprising the oily composition according to claim 1 and an emulsifier in addition to the powdered base material. 3. The powder composition according to claim 1, wherein the water-soluble film-forming agent according to claim 1 is contained in an amount of 1 to 95% by weight based on the total weight of the solid phase. 4. The water-soluble film-forming agent according to claim 3, which is one or more selected from gelatin, glue, gum arabic, starch microbial culture, hemicellulose, and a water-soluble film-forming synthetic polymer. Item 4. The powder composition according to any one of Items 1 to 3. 5. The oily composition according to claim 1, which contains 1 to 90% by weight of a polyhydric alcohol having two or more hydroxyl groups in a molecule with respect to the total weight of the solid phase. Item 5. The powder composition according to any one of Items 1 to 4. 6. The powder composition according to claim 1, wherein the oily composition according to claim 1 or 2 contains an oil-soluble active substance in an oil phase. 7. The oily composition according to claim 1, which contains 5 to 75% by weight of a solid phase and 95 to 25% by weight of an oil phase. A powder composition as described. 8. W / Emulsified water phase containing water-soluble active substance and / or water-dispersible substance, water-soluble film-forming agent and water or alcohol aqueous solution, and oil phase containing oil component and emulsifier. The powder composition according to any one of claims 1 to 7, wherein an oily composition obtained by drying the O-type emulsion is used.