Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K9/00—Medicinal preparations characterised by special physical form
  • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
  • A61K9/4841—Filling excipients; Inactive ingredients
  • A61K9/4866—Organic macromolecular compounds
• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES OF CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
  • A24D3/00—Tobacco smoke filters, e.g. filter tips or filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces of cigars or cigarettes
  • A24D3/06—Use of materials for tobacco smoke filters
  • A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
  • A23P10/00—Shaping or working of foodstuffs characterised by the products
  • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
  • A23P10/35—Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES OF CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
  • A24D3/00—Tobacco smoke filters, e.g. filter tips or filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces of cigars or cigarettes
  • A24D3/06—Use of materials for tobacco smoke filters
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
  • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
  • A61K47/14—Esters of carboxylic acids, e.g. fatty acid monoglycerides, medium-chain triglycerides, parabens or PEG fatty acid esters
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
  • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
  • A61K8/11—Encapsulated compositions
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/31—Hydrocarbons
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
  • A61K8/37—Esters of carboxylic acids
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/60—Sugars; Derivatives thereof
  • A61K8/604—Alkylpolyglycosides; Derivatives thereof, e.g. esters
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
  • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K9/00—Medicinal preparations characterised by special physical form
  • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
  • A61K9/4841—Filling excipients; Inactive ingredients
  • A61K9/4875—Compounds of unknown constitution, e.g. material from plants or animals
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q19/00—Preparations for care of the skin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q90/00—Cosmetics or similar toiletry preparations for specific uses not provided for in other groups of this subclass
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
  • B01J13/02—Making microcapsules or microballoons
  • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/10—General cosmetic use
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
  • A61K2800/41—Particular ingredients further characterized by their size

Definitions

• the present invention relates to a water-filled capsule having a water-containing core and an encapsulation layer disposed on the outside of the water-containing core, and a method for manufacturing the same.
• water-filled capsules that have excellent resistance to water evaporation are known, and include a water-containing core that contains water, an inner layer disposed on the outside of the water-containing core, and an outer layer disposed on the outside of the inner layer, in which the inner layer is made of a lipophilic material and the outer layer is made of a hydrophilic material in which lipophilic particles or water-insoluble particles are dispersed (Patent Document 1).
• a filter element for use in tobacco articles which has at least one filter body, a core material containing a liquid medium, and a capsule with a water vapor impermeable polymerized shell, the liquid medium of the core material containing at least one surfactant (Patent Document 2).
• Patent Document 3 A method for producing easily breakable raw capsules useful for incorporation into tobacco products has also been proposed (Patent Document 3).
• Oils, oil-soluble substances, and emulsions are well known as liquid contents that can be formulated in soft capsules.
• the water evaporates through the capsule membrane soon after encapsulation, making it impossible to retain the moisture of the liquid contents for the long term.
• the objective of the present invention is to provide a technology for water-filled seamless capsules that are water-resistant and capable of containing and retaining the moisture of the liquid contents within the capsule for the long term.
• the inventors have conducted extensive research to find a solution to the above problems, and have discovered that in a water-filled capsule having a water-containing core and an encapsulation layer disposed on the outside of the water-containing core, by making the encapsulation layer out of a lipophilic composition having a specific gravity within a specific range, and by maintaining the encapsulation layer at a thickness above a certain range, it is possible to encapsulate and retain the moisture in the water-containing core within the capsule for a long period of time, and by including a viscosity additive that imparts viscosity to the water in the water-containing core, it is possible to improve the formulation properties of the capsule, which has led to the completion of the present invention.
• a water-filled capsule comprising a water-containing core and an encapsulation layer disposed on the outside of the water-containing core, the encapsulation layer being made of a lipophilic composition having a specific gravity of 0.79 to 1.05, and the thinnest part of the encapsulation layer being 80 ⁇ m or more.
• the water-filled capsule according to the above [1] wherein the water-containing core contains a viscosity additive that imparts viscosity to the water.
• the lipophilic composition contains a specific gravity adjuster that adjusts the specific gravity of the lipophilic composition to 0.79 to 1.05.
• the present invention can provide three-layer water-filled seamless capsules and two-layer water-filled seamless capsules that have little change in water encapsulation rate over time when left open at room temperature, can encapsulate and retain the moisture of the content liquid (water-containing core) within the capsule for a long period of time, and have excellent water resistance.
• the physical properties of the encapsulation layer can be set according to the application of the water-filled capsule.
• the physical properties of the encapsulation layer arranged on the outside of the water-containing core can be set to be hard or soft depending on the oily substance that constitutes it. For example, if the encapsulation layer is set to be soft, the two-layer capsule design can be used as a water-filled raw capsule that can be easily crushed with fingers for use, and can be used for cosmetics and quasi-drug applications.
• the water-filled capsule of the present invention is a water-filled capsule having a water-containing core and an encapsulation layer disposed on the outside of the water-containing core, the encapsulation layer being made of a lipophilic composition having a specific gravity of 0.79 to 1.05, and the thinnest part of the encapsulation layer having a thickness of 80 ⁇ m or more.
• the water-filled capsule there are no particular limitations on the water-filled capsule, and suitable examples include two-layer water-filled capsules and three-layer water-filled capsules, but multi-layer water-filled capsules with four or more layers are also acceptable.
• the above-mentioned hydrous core is not particularly limited as long as it contains water, and may be composed of only water, but it is preferable that it contains a viscosity additive that imparts viscosity to the water, and may also contain various other active ingredients and various additives.
• the above-mentioned viscosity additives include, for example, alginic acid, alginates such as sodium alginate, alginate esters such as propylene glycol alginate, celluloses such as methylcellulose, ethylcellulose, hydroxypropylmethylcellulose, hydroxypropylcellulose, and carboxymethylcellulose, gelatin, carrageenan, agar, starch, modified starch, dextran, dextrin, pullulan, glucomannan, gum arabic, furcellaran, and tragacanthus.
• alginic acid alginates such as sodium alginate
• alginate esters such as propylene glycol alginate
• celluloses such as methylcellulose, ethylcellulose, hydroxypropylmethylcellulose, hydroxypropylcellulose, and carboxymethylcellulose
• gelatin carrageenan
• agar starch, modified starch, dextran, dextrin, pullulan, glucomannan, gum arab
• gums examples include guar gum, locust bean gum, gellan gum, xanthan gum, polyvinylpyrrolidone, polyvinyl alcohol, glucosamine, Eucheuma algae, soybean water-soluble polysaccharides, welan gum, cassia gum, Agrobacterium succinoglycan, guar gum enzymatic hydrolysate, ghatti gum, arabinogalactan, curdlan, karaya gum, tamarind seed gum, psyllium seed gum, tara gum, amas seed gum, konjac powder (potato), hydroxypropylated guar gum, and pectin.
• the oily substance constituting the lipophilic composition can be, first, an oily substance having a melting point of 20°C or higher (hereinafter referred to as "solid fats and oils").
• solid fats and oils include hydrogenated oils (liquid animal and vegetable fats and oils with a higher melting point by hydrogenating them), partially hydrogenated oils (hydrogenated oils obtained by hydrogenating only a portion of liquid animal and vegetable fats and oils, or mixtures of non-hydrogenated fats and oils and hydrogenated oils), and waxes.
• solid fats and oils include hydrogenated castor oil, hydrogenated soybean oil, hydrogenated rapeseed oil, hydrogenated coconut oil, cacao butter, butter, hydrogenated palm kernel oil, head, beef tallow hydrogenated oil, lard, lard hydrogenated oil, beeswax (beeswax), candelilla wax, rice bran wax, carnauba wax, Japan wax, urushi wax, and mixtures thereof.
• examples of oily substances constituting the lipophilic composition include liquid oily substances (hereinafter referred to as "liquid oils") having a melting point of less than 20°C, and specific examples include animal and vegetable oils such as safflower oil, linseed oil, sesame oil, olive oil, soybean oil, mustard oil, rapeseed oil, corn oil, castor oil, evening primrose oil, palm kernel oil, jojoba oil, cottonseed oil, coconut oil, peanut oil, EPA, DHA, DPA, squalane, shark liver oil, and cod liver oil, as well as medium-chain triglycerides (MCT) and liquid paraffin.
• liquid oils liquid oily substances having a melting point of less than 20°C
• specific examples include animal and vegetable oils such as safflower oil, linseed oil, sesame oil, olive oil, soybean oil, mustard oil, rapeseed oil, corn oil, castor oil, evening primrose oil, palm kernel oil, jojoba oil, cottonseed oil
• the oily substances constituting the lipophilic composition include surfactants such as glycerin fatty acid esters, sucrose fatty acid esters, and fatty acid acyl esters that are highly lipophilic (for example, those with an HLB of less than 7 or less than 10).
• surfactants such as glycerin fatty acid esters, sucrose fatty acid esters, and fatty acid acyl esters that are highly lipophilic (for example, those with an HLB of less than 7 or less than 10).
• those that are solid at 20°C can be used as solid oils and fats
• oily substances that are liquid at temperatures below 20°C can be used as liquid oils and fats.
• the lipophilic composition that can be used in the present invention may be a mixture of one or more types appropriately selected from solid oils and liquid oils and fats, and commercially available products such as the "GELUCIRE” series manufactured and sold by Gattefosse, Nissin MCT Oil, Kao “Excel” series, Kao “Econa” series, Kao “Emanone” series, and Kao “Leo D'or” series may be used.
• oily functional components oil-based components having various functions such as nutritional function, fragrance function, pigment function, etc.
• oily nutritional functional components examples include omega fatty acids such as oleic acid, linoleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid, docosahexaenoic acid, and docosapentaenoic acid, oily substances such as prostaglandins, oil-soluble vitamins such as vitamin A, vitamin E, vitamin D, and vitamin K, and oils and fats containing these.
• oily components having a fragrance function include natural essential oils such as orange oil, lemon oil, perilla oil, ambrette seed oil, orris root oil, cananga oil, mustard oil, caraway oil, carrot seed oil, grapefruit oil, ginger oil, hop oil, myrtle oil, rose oil, and rosemary oil, and synthetic or natural flavorings such as eugenol, ethyl caprylate, geraniol, menthol, citral, citronellal, and borneol.
• oily components having a pigment function include oil-based colorings such as annatto pigment, carotene, and oleoresin. Naturally, these can be used alone or in combination.
• the lipophilic composition may contain an oil-insoluble component. Any component that is miscible with an oil-based component may be used as the oil-insoluble component. Examples of oil-insoluble components that can be used with an oil-based component include inorganic powders such as titanium dioxide, calcium carbonate, magnesium carbonate, magnesium oxide, calcium stearate, magnesium stearate, (fine) silicon dioxide, and aluminum oxide.
• a specific gravity adjuster can be used to adjust the specific gravity of the lipophilic composition to a predetermined range.
• a specific gravity adjuster is a substance that can be dissolved or mixed with the lipophilic composition and has a specific gravity different from that of the lipophilic composition before the specific gravity adjuster is added.
• an oily substance having a specific gravity of 1 or more such as SAIB (Sucrose Acetate Isobutylate), wood rosin glycerin ester, sucrose octaacetate, etc., can be suitably used.
• inorganic powders such as titanium dioxide, calcium carbonate, magnesium carbonate, magnesium oxide, calcium stearate, magnesium stearate, (fine) silicon dioxide, and aluminum oxide can also be used as specific gravity adjusters if they can adjust the specific gravity by mixing with the lipophilic composition before addition.
• animal and vegetable oils, synthetic oils, ester oils, mineral oils, etc. that are acceptable for the purpose of use of the present invention can also be used as specific gravity adjusters if they can adjust the specific gravity by adding them to the lipophilic composition before addition.
• the specific gravity of the encapsulation layer in the present invention can be 0.79 to 1.05, 0.79 to 1.03, 0.79 to 1.0, 0.795 to 1.05, 0.795 to 1.03, 0.795 to 1.0, 0.8 to 1.05, 0.8 to 1.03, 0.8 to 1.0, 0.83 to 1.05, 0.83 to 1.03, 0.83 to 1.0, 0.85 to 1.05, 0.85 to 1.03, 0.85 to 1.0, with 0.80 to 1.0 being particularly preferred examples.
• water-filled capsules using a low-density lipophilic composition [e.g., a mixture of the above-mentioned squalane and hydrogenated oil, encapsulation layer specific gravity: 0.795] and a high-density lipophilic composition [e.g., a mixture of the above-mentioned SAIB and hydrogenated oil, encapsulation layer specific gravity: 1.03] as the encapsulation layer.
• a low-density lipophilic composition e.g., a mixture of the above-mentioned squalane and hydrogenated oil, encapsulation layer specific gravity: 0.795
• a high-density lipophilic composition e.g., a mixture of the above-mentioned SAIB and hydrogenated oil, encapsulation layer specific gravity: 1.03
• the thickness of the encapsulation layer what is important is the thickness of the thinnest part (thinnest part thickness), and as long as it is kept at a minimum level, for example 80 ⁇ m or more, preferably 90 ⁇ m or more, 100 ⁇ m or more, 110 ⁇ m or more, 120 ⁇ m or more, 150 ⁇ m or more, 180 ⁇ m or more, 210 ⁇ m or more, 240 ⁇ m or more, 270 ⁇ m or more, 300 ⁇ m or more, 350 ⁇ m or more, 400 ⁇ m or more, 450 ⁇ m or more, 500 ⁇ m or more, there may be some bias in the thickness.
• a three-layer water-filled capsule can be formed by providing an additional membrane layer on the outside of the above-mentioned encapsulation layer.
• a membrane layer may be any layer that is commonly used as a membrane for seamless capsules, and examples of such a membrane layer include gelatin, casein, zein, pectin and its derivatives, alginic acid or its salts, agar, gellan gum, tragacanth gum, guar gum, locust bean gum, carrageenan, tamarind, mannan, hemilose, starch, chitosan, etc., as a base.
• the membrane layer may also contain, in addition to the base, plasticizers such as glycerin, sorbitol, propylene glycol, and polyethylene glycol, pH adjusters such as sodium phosphate, chelating agents such as trisodium citrate and sodium metaphosphate, gelation promoters such as calcium lactate and potassium chloride, surfactants such as polyglycerin fatty acid esters and lecithin, sweeteners, flavorings, preservatives, colorants, etc.
• the above-mentioned coating layer may contain additives such as natural dyes, synthetic dyes, various sweeteners, preservatives, water activity reducing agents, pH adjusters, etc. It is also possible to classify the three-layer water-filled capsules into dry capsules and raw capsules based on the water content of the above-mentioned coating layer.
• the coating liquid used for the above coating layer is preferably one with a viscosity of 300 mPa ⁇ s or less at 85°C, measured using a C-type viscometer (Toki Sangyo Co., Ltd., VISCOMETER TVC-7) with rotor No. 1 (upper limit 500 mPa ⁇ s).
• the method for producing the water-filled capsules of the present invention is not particularly limited as long as it uses a concentric triple nozzle, extruding the water-containing core from the inner nozzle, the encapsulating layer from the middle nozzle, and the coating layer from the outer nozzle to form three-layer droplets, and then contacting the three-layer droplets with a cooling solvent set at, for example, 0 to 25°C to form water-filled pre-capsules.
• the cooling solvent include cooling oils such as MCT composed of fatty acids such as capric acid and caprylic acid, liquid paraffin, vegetable oils such as sunflower oil and safflower oil, or mixtures of these, and low-temperature gases such as air, helium, nitrogen, and argon.
• a two-layer water-filled capsule can be produced, consisting of a water-containing core and a coating layer disposed on the outside of the water-containing core. Since the coating layer is soft, it can be peeled off easily with a simple tool such as a finger or a medicine spoon before the water-filled pre-capsule dries.
• the water-filled capsules of the present invention are two-layer water-filled capsules, they can be roughly divided into solid capsules and raw capsules depending on the hardness of the encapsulation layer.
• the hard encapsulation layer is solid capsules
• the soft encapsulation layer is raw capsules.
• a rheometer was newly used to measure the hardness of each encapsulation layer formulation and compare the maximum loads.
• capsules formed with an encapsulation layer of 5 kg or less in maximum load when the adapter is pushed 3 mm into the rheometer using the following [measurement equipment] [measurement method] will be classified as two-layer water-filled raw capsules (two-layer raw capsules) and capsules formed with an encapsulation layer of more than 5 kg in maximum load (two-layer solid capsules).
• a solid oil or a solid oil and a liquid oil is used as an example of the lipophilic composition of the encapsulation layer
• the melting point (actual value) of the encapsulation layer is, for example, 37°C or higher
• the specific gravity of the encapsulation layer is, for example, 0.82 to 1.05.
• a mixed oil of a solid oil and a liquid oil is used as an example of the lipophilic composition of the encapsulation layer
• the melting point (actual value) of the encapsulation layer is, for example, 16 to 36.8°C
• the specific gravity of the encapsulation layer is, for example, 0.79 to less than 0.82.
• a two-layer raw capsule is usually an easily disintegrating capsule. It was found that the melting point of the encapsulation layer, which is a mixture of a solid oil and a liquid oil, does not show a double peak of the melting points of the solid oil and the liquid oil, but shows almost a single peak.
• the melting point was measured using a differential scanning calorimeter "DSC7020” (Hitachi High-Tech Science Corporation), starting at 0°C and increasing the temperature at 5°C/min, with the endothermic peak being the actual measured melting point.
• DSC7020 Different scanning calorimeter
• the melting point of the oily substance constituting the lipophilic composition is not particularly limited, but when the water-filled capsule is a two-layer capsule, it can be roughly classified as either a solid capsule or a raw capsule depending on the properties of the lipophilic composition. That is, in the case of a two-layer solid capsule, the lipophilic composition has a melting point of 20°C or higher, preferably 30°C or higher, and preferably has a melting point of 100°C or lower, preferably 80°C or lower, more preferably 70°C or lower, and among these, a lipophilic composition having a melting point of 30°C to 70°C can be preferably exemplified.
• the lipophilic composition can also be appropriately adjusted by mixing multiple oily substances such as hardened oils with different melting points, or by adding liquid animal and vegetable oils.
• the water-filled capsule has the properties of a raw capsule, for example, a mixture of the above-mentioned solid oil and fat and a liquid oil with a melting point of less than 20°C is used.
• the melting point of the mixed oil in the encapsulating layer is 16°C, even if it is liquid at room temperature, it will remain semi-raw under refrigerated conditions, and if distribution and use under refrigerated conditions are considered, it can also be considered a two-layer raw capsule.
• the water-filled capsule when it is a three-layer capsule, it can be roughly classified as either a raw capsule or a dry capsule, mainly depending on the properties of the coating.
• the above-mentioned concentric triple nozzle is used to eject the water-containing core from the inner nozzle, the encapsulation layer from the middle nozzle, and the coating layer from the outer nozzle to form three-layer droplets, and the water-filled pre-capsules formed by contacting these three-layer droplets with a cooling solvent are prepared into three-layer raw capsules without going through a coating drying process, which is a major feature of the capsules.
• step refers to producing a three-layer water-filled capsule without using known means for drying capsules such as spray drying, freeze drying, air drying, vacuum drying, static drying, vacuum vibration drying, etc., but for convenience, it can also include stopping the drying step (drying stop step) before the water content ratio (moisture content) of the shell of the water-filled pre-capsule becomes, for example, less than 20%, less than 25%, less than 30%, less than 45%, less than 70%, or less than 90%.
• the moisture content of the shell of a three-layered raw capsule can be 20% or more, preferably 25% or more, more preferably 30% or more, more preferably 45% or more, even more preferably 70% or more, and even more preferably 90% or more.
• the three-layered capsule shells that do not undergo the above-mentioned drying process are characterized by their softness, and the moisture content of the shells can be measured, for example, using an infrared moisture meter FD-720 (Kett Electric Laboratory) under conditions of 1 g of shell/105°C/15 minutes.
• the above three-layered raw capsule can be produced and stored by a method comprising the following steps (a) to (c): (a) forming a triple-layer droplet using a concentric triple nozzle, discharging a water-containing core from an inner nozzle, an encapsulating layer from a middle nozzle, and a coating layer from an outer nozzle; (b) contacting the trilayer droplets with a cooling solvent to form water-encapsulated precapsules; (c) immersing the water-filled precapsules in a capsule preservation solution;
• the three-layer water-sealing capsule can be washed with detergent or with running water, if necessary, to remove the cooling solvent adhering to the periphery.
• the capsule preservative may be an aqueous solvent containing at least one water selected from tap water, well water, distilled water, purified water, ion-exchanged water, ultrapure water, deep ocean water, mineral water, etc., but since the water content of the capsule is high, for example, when cosmetics are used, a preservative such as phenoxyethanol or an antibacterial agent such as 1,3-butylene glycol may be added to the capsule or preservative to prevent spoilage of the capsule.
• the three-layer raw capsule thus obtained can be immersed in a preservative and transported, and is excellent in that the encapsulated water and water-soluble components can be sealed and maintained in the capsule for a long period of time even during storage and transportation in the raw capsule state.
• one example of the uses of the three-layer raw capsule is its use in a form in which it is mixed and dispersed in a product that is rich in water, and it is expected that the fields of use will be diverse, including food, medicines, quasi-drugs, cosmetic compositions such as cosmetics, topical skin preparations, beverages, pet food, and luxury items.
• a capsule can be prepared by drying the above-mentioned water-filled pre-capsules using known capsule drying methods such as spray drying, freeze drying, air drying, vacuum drying, static drying, vacuum vibration drying, etc., to produce a triple-layered dry water-filled capsule (triple-layered dry capsule).
• the moisture content in the shell of the triple-layered dry capsule can be less than 20%, preferably 15% or less, more preferably 10% or less, and even more preferably 8% or less.
• the three-layer dry capsule can be produced by a method comprising the following steps (a) to (c): (a) forming a triple-layer droplet by using a concentric triple nozzle, ejecting a water-containing core from an inner nozzle, the encapsulating layer from a middle nozzle, and the coating layer from an outer nozzle; (b) contacting the trilayer droplets with a cooling solvent to form water-encapsulated precapsules; (c) drying the water-filled pre-capsules to prepare three-layer dry capsules;
• the hardness of the capsule shell is 0.5-40N, preferably 0.5-20N, from the viewpoints of manufacturability and fragility
• the thickness of the capsule shell is 20-500 ⁇ m, preferably 40-200 ⁇ m
• the diameter of the capsule is 0.5-15mm, preferably 1-8mm, from the viewpoints of ease of gripping and content volume
• the capsule shell ratio is 5-30%, for example.
• the three-layer dry capsule can be easily broken by hand, and the snapping sound and feel that occurs when the capsule is broken are pleasant. Therefore, if a capsule containing flavorings is embedded inside a filter that comes with a cigarette or a filter to be attached to a cigarette, the recipient can crush the capsule with their fingers while smoking to obtain the sound, feel, and aroma of the capsule being crushed. Also, if a capsule containing flavorings is placed on a greeting card, the recipient can crush the capsule to obtain the sound, feel, and aroma.
• the present invention can be applied to daily necessities such as medicines, health foods, foods, cosmetics, and cleaning supplies.
• the three-layer dry membrane capsule may include not only the easily breakable capsules used for tobacco applications as described above, but also capsules suitable for oral intake.
• the water encapsulation stability of the capsule of the present invention can be determined by measuring the mass of the capsule left open at 22°C and 18-45% RH (or 70% RH at 5°C, or 8% RH at 25°C) to measure the change in the water encapsulation rate over time, and judging that the capsule has water encapsulation stability if the water encapsulation rate is 75% or more, preferably 85% or more, and more preferably 90% or more after 4 weeks, and 50% or more, preferably 75% or more, more preferably 78% or more, even more preferably 80% or more, and especially preferably 90% or more after 8 weeks.
• An example of a method for evaluating the water resistance of the capsules of the present invention is to visually check for pigment transfer to the hydrous core when the capsule is immersed in a preservation solution and stored.
• the preservation solution remains colorless and does not change color, but when the water and water-soluble components in the hydrous core transfer to the preservation solution through the membrane, the preservation solution turns blue, and it can be visually confirmed that the solution is unstable.
• the outermost gelatin coating layer of the above three-layer water-filled pre-capsule was peeled off without going through a drying process to produce a two-layer water-filled capsule. It has been confirmed that water can be filled in as long as the filling layer of this two-layer water-filled capsule exists as the outer layer, and that the gelatin coating layer is not necessarily required.
• Examples 1 to 7 In the hydrous cores of Examples 1 to 6, the water is thickened with sodium alginate, Chimica Algin IL-2 (manufactured by Chimica Co., Ltd.), to improve filling properties.
• the encapsulation layer is based on four types of solid fats and oils, and the thickness of the encapsulation layer exceeds 70 ⁇ m, making it possible to encapsulate water.
• SAIB specific gravity adjuster
• the water inclusion rate test shown in Table 2 measured the change in water inclusion rate over time after 4, 8, 12, and 16 weeks of exposure to open conditions at 22°C and 18-45% RH (or 70% RH at 5°C and 8% RH at 25°C).
• 100% water was filled into Comparative Example 1 [polyethylene bag: made of low-density polyethylene resin, thickness 0.06 mm] and Comparative Example 2 [rubber balloon (water balloon): made of natural rubber, thickness 0.10 mm], and the change in water inclusion rate over time was measured.
• Comparative Example 1 was superior to Comparative Example 2 in terms of water inclusion rate, and Examples 1 to 7 had water inclusion rates that were roughly equivalent to or better than Comparative Example 1.
• Example 4 the capsules of Example 4-1 were obtained by seamlessly filling three layers, and then the outer gelatin coating layer was peeled off without going through a coating drying process to produce two-layer water-filled capsules.
• Water can be filled in as long as the encapsulation layer is present as the outer layer, and the coating layer (gelatin) is not necessarily required.
• the presence or absence of a coating layer is appropriately selected depending on the product application.
• the results of the change in water encapsulation rate over time in Examples 4 and 4-1 show that there is no difference in the water encapsulation rate between the two-layer and three-layer structures.
• Examples 8 to 12 In Examples 8 to 12 and Comparative Example 3, in order to grasp the thinnest thickness of the encapsulation layer capable of encapsulating water, two-layer capsules were prepared in which the thinnest thickness of the encapsulation layer was varied from 700 to 70 ⁇ m, and the change in the water encapsulation rate over time was measured after 4 weeks, 8 weeks, 12 weeks, and 16 weeks when left open at 22° C. and 18 to 45% RH. To measure the thickness of the thinnest part of the encapsulation layer, a high-resolution 3D X-ray microscope "NANO3DX" (manufactured by Rigaku Corporation) was used to take non-destructive cross-sectional images to confirm the film thickness.
• NANO3DX manufactured by Rigaku Corporation
• Each water-filled capsule was prepared according to the formula shown in Table 4 below.
• Examples 13 and 14 In the water-filled capsules of Examples 13 and 14, the encapsulation layer was made of an oily material containing a mixture of solid oil and squalane, a liquid oil having a melting point of -38°C, and the specific gravity of the encapsulation layer was set to a low specific gravity of 0.795 and 0.815, respectively.
• the maximum load measured by a rheometer was 0.75 kg in Example 13 and 3.42 kg in Example 14, and two-layered water-filled raw capsules with a soft encapsulation layer were obtained.
• the data after 8 weeks of the water-filling rate aging test showed that both of the two-layered raw capsules maintained a water-filling rate superior to that of Comparative Example 2 (rubber balloon (water balloon)). Therefore, it was confirmed that the two-layered raw capsules with an encapsulation layer specific gravity of 0.795 to 0.815 maintained an excellent water-filling rate.
• Example 15 and 16 In the water-filled capsules of Examples 15 and 16, the encapsulation layer was made of an oily material made of a mixture of solid oil and liquid oil squalane, and the specific gravity of the encapsulation layer was set to be slightly high at 0.825 or 0.835. The maximum load measured by a rheometer was 5.81 kg in Example 15 and 7.18 kg in Example 16, and two-layered water-filled solid capsules were obtained with the encapsulation layer set to be relatively hard.
• Example 17 The specific gravity of the lipophilic composition in the encapsulation layer was set to a high specific gravity of 0.99 using SAIB as a specific gravity adjuster, and the two-layer solid capsule was prepared as Example 17. The data after 8 weeks of the water encapsulation rate aging test showed that the water encapsulation rate was superior to that of Comparative Example 2 (rubber balloon (water balloon)).
• Example 18 a triple-layered dry capsule with a gelatin-based film was prepared with a high specific gravity of 0.99.
• a triple-layered dry capsule with a gelatin-based film was prepared with an even higher specific gravity of 1.03.
• water-containing core water, propylene glycol, and/or ethanol, and/or glycerin were used as components of the water-soluble fragrance.
• hydroxypropyl cellulose was used as a viscosity additive instead of sodium alginate, which was previously used.
• SAIB was used as a specific gravity adjuster in the encapsulation layer, and the specific gravity of the encapsulation layer was set high at 0.94 or 0.945.
• a carrageenan-based coating formulation containing carrageenan and water a gelatin-based coating formulation containing gelatin and water, or an agar-based coating formulation containing agar and water was used, which can be used in capsules for embedding in cigarette filters and cartridges for masks.
• Example 20 to 25 The six types of three-layered dry capsules in Examples 20 to 25 all had a thinnest film thickness in the range of 130 ⁇ m to 300 ⁇ m.
• the specific gravity of the encapsulation layer using a solid oil with a melting point of 44.2°C and a specific gravity adjuster SAIB was 0.940 to 0.945, but the physical properties of the encapsulation layer became hard, resulting in a three-layered dry water-filled capsule.
• the membrane layer was carrageenan-based, gelatin-based, or agar-based, it could be easily broken with fingers, and the snapping sound and feel generated when the capsule was broken were pleasant and good.
• the moisture content of the coating layer of the six types of dry capsules was measured using an infrared moisture meter FD-720 (Kett Electric Laboratory) under conditions of 1 g of coating/105°C/15 minutes, and was in the range of 8-15% for all of them.
• the thickness was 40-200 ⁇ m, the hardness was 0.5-20 N, the coating rate was 5-30%, and the capsule diameter was 1-8 mm.
• the raw capsules in the prior art are two-layer capsules in which an oil-soluble component or a lipophilic composition is encapsulated in a soft, wet membrane, and are known to be used in cosmetics.
• the capsule is ground to break the capsule membrane, and the contents released at the application site are mixed in a fresh state with a cosmetic base in a liquid, cream, or semi-solid form.
• the contents generally used are oil-soluble components or lipophilic compositions, and no raw capsules containing water or water-soluble components are known. Therefore, we decided to study a three-layer raw capsule having a water-containing core that is intended for use as described above (Examples 26 to 30).
• Blue No. 1 was added to the water as a pigment to visually confirm the pigment transfer in the hydrated core during the water resistance test, and sodium alginate was used as a viscosity additive.
• the specific gravity of the encapsulation layer was high because MCT (Coconard MT, manufactured by Kao) was used as a liquid oil in addition to the solid oil in the encapsulation layer.
• MCT Coconard MT, manufactured by Kao
• SAIB was used as a specific gravity adjuster, and the specific gravity of the encapsulation layer was set high at 1.01 and 1.00.
• the thinnest film thickness was 150 ⁇ m or more in all cases.
• a carrageenan-based coating formulation containing carrageenan and water a gelatin-based coating formulation containing gelatin and water, or an agar-based coating formulation containing agar and water was used.
• Examples 26 to 30 (Checking water resistance)
• the three-layer capsules of Examples 26 to 30 were three-layer capsules containing raw water, with the thinnest part of the encapsulation layer having a thickness of 150 ⁇ m or more, and the specific gravity of the encapsulation layer using MCT as the liquid oil being 0.930 to 1.010.
• MCT the specific gravity of the encapsulation layer using MCT as the liquid oil
• the measured values of the water content of the shell of the three-layer raw capsules were 20.4% for the carrageenan-based shell capsule, 49.6% for the gelatin-based shell, and 97.5% for the agar-based shell capsule, and it was determined that the shells were soft and were raw capsules at these water contents.
• the thinnest part of the encapsulation layer had a thickness of 60 ⁇ m, but after 8 weeks, all capsules leaked dye, and water resistance was not obtained.
• the thinnest part of the encapsulation layer had a thickness of 200 ⁇ m or more
• the thinnest part of the encapsulation layer had a thickness of 500 ⁇ m or more, and the water in the glass vial was not colored blue even after 16 weeks, and the capsules had water resistance without dye leakage.
• Example 33 which has an encapsulation layer with a thinnest part thickness of 500 ⁇ m or more, the gelatin film layer swells over time, but there is no dye leakage from the water-containing core, and the capsules were water-resistant.
• the specific gravity of the encapsulation layer was set to 0.940 and 1.030, respectively, and good water resistance was obtained.
• the water-filled capsule of the present invention can be used as a water-filled capsule that can stably retain hydrophilic volatile substances for long periods of time in pharmaceuticals, quasi-drugs, cosmetics, food, beverages, dairy products, seasonings, supplements, pet food, household products, luxury items such as tobacco and tobacco substitutes, industrial products such as fertilizers, feed, and cleaning agents, and other fields.

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• 2023
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