Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
  • A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
  • A61J3/07—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use
  • A61J3/071—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use into the form of telescopically engaged two-piece capsules
  • A61J3/077—Manufacturing capsule shells
• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
  • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for 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
  • 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
  • A61K9/4816—Wall or shell material

Definitions

• the present invention relates to a soft capsule having carrageenan in the composition of the capsule shell and a method for producing the same.
• Soft capsules are widely used in the fields of medicines, cosmetics, health foods and the like.
• its use has been expanded, and not only a technique for increasing the strength of the capsule film to make it hard to break but also a technique for making it easy to break, as in the past, has been sought.
• As a use of the technique to make it easy to break for example, burying the capsule which contains the perfume etc in the filter of the cigarette, breaking the capsule at the time of smoking etc to enjoy the smell and enjoying the sound and feel when the capsule breaks Etc.
• the technique to make it easy to break for example, burying the capsule which contains the perfume etc in the filter of the cigarette, breaking the capsule at the time of smoking etc to enjoy the smell and enjoying the sound and feel when the capsule breaks Etc.
• Patent Document 1 discloses that, in a soft capsule having a joint, the bonding surface of the joint is inclined, or a special mold is used to provide a fringe to thicken only the bonding portion.
• Patent Document 2 discloses that, in a jointed soft capsule for a bath agent, suppression of local thinning of a bonded part of a film is disclosed.
• thinning the capsule shell lowers the hardness, the capsule shell deforms comfortably without cracking because the capsule shell itself has adequate plasticity.
• carrageenan As a gelling agent for films.
• carrageenan has a high thickening effect and a high gelation rate, containing a large amount of carrageenan hinders encapsulation. That is, when the content of carrageenan is high, due to high viscosity and quick gelation, the formability of the capsule is bad, such as sphericity is bad and easiness of solidification at the tip of the injection nozzle, and preferred capsule could not be manufactured .
• carrageenan is blended with starch, dextrin, non-gelling polysaccharide or the like as a base or filler to increase the solid content concentration of the film to lower viscosity and gelation. It is disclosed to reduce the speed.
• starch, dextrin, and non-gelling are often used even when carrageenan, which is considered to be less hygroscopic than gelatin, is adopted for the film.
• saccharides and the like are blended, they are easily affected by humidity, and it is not possible to stably obtain temporally stable added value such as fragility with fingers after drying and sound and feel at the time of cracking.
• Patent Documents 4 to 5 also disclose a capsule shell having a high content of carrageenan, but there is no particular mention of the function and effect thereof.
• Patent Document 4 describes that sodium citrate and the like and a carbonate neutralizer and the like are used, and the acid promotes the decomposition of carrageenan, but the neutralizer is disclosed as one that suppresses the deterioration. It has stayed.
• patent document 6 describes adding potassium citrate etc. to carrageenan, it is only indicated as what adjusts viscosity and elasticity.
• Patent Documents 7 to 14 disclose that the capsule is embedded in a filter of cigarette, but the manufacturability of the capsule, the preservability, the easiness of cracking with fingers after drying, the sound at the time of cracking, The added value such as feeling is not considered.
• Patent Document 1 Japanese Patent Application Laid-Open No. 2001-288075 JP-A-5-51315 US6214376 B1 Special Feature 2002-517378 JP 2007-526210
• Patent document 1 JP 2008-235752 Special table 2009-504175 Special Table 2008-528053 Special feature 2008-546400 JP 2008-43347 Special Feature 2007-507230 Special Features 2007-520204 Japanese Patent Application Publication No. 2003-304856 JP-A-64-60363
• the present invention maintains the hardness by increasing the content of carrageenan in the composition of the capsule shell, but relaxes the thickening effect and gelation rate by carrageenan, and stabilizes the manufacturability of the capsule and preserves it.
• An object of the present invention is to provide a soft capsule which can obtain added value such as a crack easily with fingers after drying and a sound and a feeling when cracking and a manufacturing method thereof.
• the soft capsule of the present invention is characterized in that the composition of the capsule shell at least contains carrageenan, an acidic pH adjuster, and a neutralizing agent.
• the composition of the capsule shell may contain any of a plasticizer, an alginate, a saccharide, a dextrin, a starch, and a processed starch.
• plasticizers contribute to the improvement of formability
• alginates contribute to the improvement of the durability to humidity.
• the alginate may be merely added, but may be subjected to a gelling treatment in an aqueous solution containing calcium ions.
• carrageenan it may be made to contribute to improvement of moldability using what viscosity was adjusted by decomposition with an acidic pH regulator.
• the content of carrageenan in the composition of the capsule shell may be 50% or more, preferably 70% or more.
• this content rate is a value except water.
• the coating rate may be 5 to 20%, preferably 7 to 15%.
• this film ratio is a ratio of the mass of the capsule film to the whole capsule.
• the thickness of the capsule coating may be 40 ⁇ m or less, preferably 30 ⁇ m or less.
• the hardness of the capsule shell is preferably 5 to 40 N. If it is smaller than 5N, it tends to cause inconvenience during the manufacturing process, and if it exceeds 40N, it becomes difficult to crush with a finger. More preferably, it may be 10 to 20N.
• the hardness measurement in this case can use a general "Kiya type hardness meter.”
• the "Kiya-type hardness tester” is to place a sample on a sample table, gradually lower a cylindrical presser from above, and record the pressure when it ruptures. In the examination in the present invention, "Kiya type digital hardness tester KHT-20N type manufactured by Fujiwara Seisakusho Co., Ltd.” was used.
• This apparatus is of a type in which a cylindrical presser descends at a constant speed electrically, and has an elevation speed of 1 mm / sec, a diameter of 5 mm of a pressure surface, and a diameter of 25 mm of a sample stage.
• the diameter of the capsule is preferably 0.5 to 15 mm. If it is smaller than 0.5 mm in diameter, it becomes difficult to grasp because it is crushed with a finger. If the diameter is more than 15 mm, the internal volume is increased, and there is a risk of contaminating the surroundings when crushed with a finger. More preferably, it may be 1 to 8 mm.
• the seamless capsule can be produced, for example, by a conventionally known dropping method.
• a typical example of the dropping method is using a concentric double nozzle, a coating liquid containing an aqueous solution of gelling agent and the like from the outer nozzle, a content from the inner nozzle simultaneously as double droplets, and the coating liquid as a gel.
• the solution is dropped into the solution to be solidified, and the outer film solution is gelled and cured to form a capsule film, thereby forming a seamless capsule without seams.
• liquid hardening method or orifice method instead of double nozzles, it is also possible to use triple or more multiple nozzles.
• the excess viscosity may be suppressed by setting the content of alginate to 50% or less of carrageenan.
• Coatings consisting of waxes or waxes may be applied to contribute moisture resistance.
• the method for producing a soft capsule according to the present invention comprises the steps of: decomposing carrageenan, which is the composition of the capsule coating, with an acidic pH adjuster; and stopping the decomposition with a neutralizing agent in the method of preparing the coating. It features. That is, the decomposition by the acid reduces the molecular weight and the viscosity, and the neutralization by the alkali stops the decomposition to set the desired viscosity.
• the degree of degradation of carrageenan may be adjusted to a preferable viscosity depending on the contents of the capsule.
• the preferable viscosity in this case is 30 to 150 mPa ⁇ s, more preferably 50 to 100 mPa ⁇ s.
• rotor No In the viscosity measurement, if the liquid temperature is 75 ° C. and the viscosity is 100 mPa ⁇ s or less with “C-type viscometer C type C made by Tokimec Co., Ltd.”, rotor No. When 0 is used, and when it exceeds 100 mPa ⁇ s, rotor No. 1 is used. It can be measured using 1.
• Alginates may be added as a composition of the capsule shell, and the alginates may be gelled in an aqueous solution of a gelation aid containing calcium ions to contribute to moisture resistance.
• An aqueous solution of gelation aid may be used containing ethanol to contribute to washing of the capsule.
• carrageenan can be adjusted to the desired viscosity by decomposing it with an acidic pH adjuster and stopping its decomposition with a neutralizing agent.
• the rate of gelation by carrageenan is also relaxed, and the processability of the capsule can be stabilized.
• the hardness can be maintained by increasing the content of carrageenan, and it is possible to provide added value such as sound and feel when the finger is easily broken and broken.
• the soft capsule according to the present invention comprises at least a carrageenan, an acidic pH adjuster, and a neutralizing agent in the composition of the capsule shell.
• the main component carrageenan can be subdivided according to the type of ⁇ , ⁇ , ⁇ , etc. or raw materials, but basically, of these, ⁇ type is essential, and both ⁇ and ⁇ can be appropriately used. .
• purified carrageenan, processed Eugema algae and Eugema algae are defined as carrageenans usable as food additives, but any of these can be used, and use as food additives
• there are many that have gelatin as a main component but those having carrageenan as a main component have advantages such as low adhesion and little influence by humidity.
• carrageenan is characterized by its high thickening effect and quick gelation. Therefore, when the content is increased, it is difficult to mold the capsule, such as solidification near the injection nozzle and deterioration of sphericity. become. On the other hand, when the content is reduced, the solid content of the film decreases, the capsule strength decreases, and disadvantages such as inability to withstand the drying process occur. Also, in general, if the coating rate is low, molding of the capsule becomes difficult.
• the inclusion of any one or both of the inorganic acid and the organic acid and various cations improves the problems caused by carrageenan, and the obtained capsule has a humidity condition
• the hardness was 40 N or less without a constant hardness, and it could be easily broken with fingers, and the sound and feel of the snapping that occurred when the capsule broke became comfortable.
• a substantially spherical seamless capsule can be obtained, preferred molding is easy in view of aesthetics.
• the content of carrageenan in the composition of the capsule shell is 50% or more, preferably 70% or more.
• the film ratio is as low as 5 to 20%, preferably 7 to 15%. Even with such a low coating ratio, good capsules free of rupture and deformation were obtained in the drying process and the transportation process.
• the capsule coating has a hardness of 5 to 40 N, preferably 10 to 20 N, and the capsule coating has a thickness of 40 ⁇ m or less, preferably 30 ⁇ m or less, in terms of manufacturability and fragility, etc. From the point of point of view, the diameter of the capsule is suitably 0.5 to 15 mm, preferably 1 to 8 mm.
• the production of soft capsules includes the steps of decomposing carrageenan, which is the composition of the capsule shell, with an acidic pH adjuster, and stopping the degradation with a neutralizing agent. That is, the molecular weight and the viscosity are reduced by the acid decomposition, and the decomposition is stopped by the alkali neutralization to set the desired viscosity.
• the degree to which carrageenan is decomposed is adjusted to a desirable viscosity by, for example, the balance with the contents of the capsule.
• acidic pH adjusters examples include citric acid, malic acid, acetic acid, formic acid, oxalic acid, lactic acid, phytic acid, hydrochloric acid, etc., weak acids, strong acids, organic acids, inorganic acids, of course, potassium hydrogen phosphate, etc. Any solution that can convert the solution of the area to an acid area can be used.
• an alkali corresponding to the acidic pH adjusting agent to be used can be used, for example, one capable of neutralizing a solution in an acidic region, such as dipotassium hydrogen phosphate, sodium citrate, sodium hydrogen carbonate and the like You can use anything.
• plasticizer is added to improve formability.
• Preferred plasticizers include glycerin, polyhydric alcohols such as polyethylene glycol, propylene glycol and polypropylene glycol, glucose, monosaccharides such as fructose, glucose and galactose, sucrose, maltose, trehalose, coupling sugar and the like 2
• Sugars and oligosaccharides, polysaccharides such as pullulan, gum arabic, arabinogalactan and cellulose, and sugar alcohols such as sorbitol, maltitol, lactitol, palatinit, xylitol, mannitol, galactitol and the like can be mentioned.
• alginate may be included.
• Alginates include alginic acid, sodium alginate, potassium alginate, ammonium alginate and the like.
• the alginate contained in the capsule may be subjected to a gelation treatment in an aqueous solution containing calcium ions (eg, an aqueous solution of calcium chloride, an aqueous solution of calcium lactate, etc. hereinafter referred to as an aqueous solution of gelling aid).
• calcium alginate is not suitable for use as a raw material, it can be changed from various alginates to calcium alginate by subsequent reaction with calcium ions in the aqueous solution of gelation aid, so in the final capsule May be included.
• alginic acid salt is not an essential component, and is merely an optional additive for the purpose of preventing moisture absorption.
• any method of said (1) (2) (3) is applicable to the method of making the alginate contained in the capsule gel in this invention, the method of said (3) is optimal.
• the immersion treatment time in the case of treatment by the method (3) is not particularly limited, but the effect is not enhanced even if the treatment is carried out for a long time, so 10 minutes or less is preferable, and 1 to 3 minutes. The degree is most preferred.
• the aqueous solution of gelation aid may be any solution that generates calcium ions when made into an aqueous solution, for example, calcium chloride aqueous solution, calcium lactate aqueous solution, calcium hydrogencarbonate aqueous solution, calcium acetate aqueous solution, calcium nitrate aqueous solution, etc. Can.
• the optimum aqueous solution concentration when using a calcium chloride aqueous solution is 1% by mass or less.
• the aqueous solution of gelation aid may contain ethanol.
• the washing step of the capsule can also be performed, which enhances the convenience of the production.
• blends an alginate is not specifically limited, It is preferable that it is 50% or less of mass of carrageenan. If the content of alginate is too high, the viscosity may increase and may affect the moldability of the capsule.
• coating may be performed with various coating agents such as waxes and waxes described later.
• a coating method a method in which a dried or dried capsule is sprayed or coated with a solution or solution of a coating agent dissolved or dispersed in a volatile solvent or the like to volatilize the volatile solvent (overcoating method), a coating agent is a volatile solvent or the like Immerse the dried capsule in a solution dissolved or dispersed in water, and volatilize the volatile solvent (dip method).
• an emulsifying agent may be appropriately blended in order to enhance the dispersibility and the suspension.
• dextrins, starch, processed starch or the like may be added as a base to adjust the susceptibility to cracking. Conversely, dextrins, starches and processed starches may not be added at all.
• the capsule can contain various things. Below, what can be contained in a capsule is illustrated. Each of these components can be contained in any part in the capsule.
• Waxes and waxes such as shellac wax, beeswax, carnauba wax, spermaceti wax, lanolin, liquid lanolin, reduced lanolin, hard lanolin, cyclic lanolin, lanolin wax, cannollola wax, mokurow, montan wax, shellac wax, rice wax, etc. It is.
• a hardened oil a plant hardened oil obtained by hydrogenating vegetable oil and fat, a beef tallow hardened oil, a pork fat hardened oil and the like can be contained.
• mineral oil liquid paraffin, petrolatum, paraffin, ozoceride, ceresin, microcrystalline wax etc. can be contained.
• fatty acids lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, linoleic acid, conjugated linoleic acid, linolenic acid, docosahexaenoic acid, eicosapentaenoic acid, 12-hydroxystearic acid, undecylenic acid, tall oil Natural fatty acids such as lanolin fatty acids, synthetic fatty acids such as isononanoic acid, caproic acid, 2-ethylbutanoic acid, isopentanoic acid, 2-methylpentanoic acid, 2-ethylhexanoic acid, isopentanoic acid and fats and oils containing these fatty acids as fatty acid compositions Etc. can be contained.
• vitamin A retinol, retinal (vitamin A1), dehydroretinal (vitamin A 2), carotene, lycopene (provitamin A), vitamin B: flusultiamine, thiamine hydrochloride, thiamine sulfate (vitamin B1 ), Riboflavin (vitamin B2), pyridoxine (vitamin B6), cyanocobalamin, methylcobalamin (vitamin B12), folates, nicotinic acids, pantothenic acids, biotins, choline, inositols, vitamin C group: ascorbic acid or derivatives thereof, Vitamin D: Ergocalciferol (Vitamin D2), Cholecalciferol (Vitamin D3), Dihydrotachysterol, Vitamin E: Vitamin E or derivatives thereof, Ubiquinones, Vitamin K: Phytonadione Min K 1), menaquinone (vitamin K 2), menatetrenone,
• capsicum tincture As a stimulant, capsicum tincture, capsicum oil, nonylic acid vanilamide, cantalicinoic acid, camphoricus tincture, camphor oil, peppermint oil, 1-menthol, camphor, benzyl nicotinate and the like can be contained.
• Benzophenone derivatives (2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid, sodium 2-hydroxy-4-methoxybenzophenone-5-sulfonate, dihydroxydimethoxyphen) as ultraviolet light absorbing or blocking agents
• Benzophenone, dihydroxydimethoxybenzophenone-sodium sulfonate, 2,4-dihydroxybenzophenone, tetrahydroxybenzophenone etc. paraaminobenzoic acid derivatives (paraaminobenzoic acid, ethyl paraaminobenzoate, glyceryl paraaminobenzoate, amyl paradimethylaminobenzoate, para Octyl dimethylaminobenzoate etc.), methoxycinnamic acid derivatives (ethyl paramethoxycinnamate, isopropyl paramethoxycinnamate, octyl paramethoxycinnamate,
• paraaminobenzoic acid derivatives As a whitening agent, paraaminobenzoic acid derivatives, salicylic acid derivatives, anthranilic acid derivatives, coumarin derivatives, amino acid compounds, benzotriazole derivatives, tetrazole derivatives, imidazoline derivatives, pyrimidine derivatives, dioxane derivatives, camphor derivatives, furan derivatives, pyrone derivatives, nucleic acids Derivative, allantoin derivative, nicotinic acid derivative, vitamin C or derivative thereof (vitamin C phosphate ester magnesium salt, vitamin C glucoside, etc.), vitamin E or derivative thereof, kojic acid or derivative thereof, oxybenzone, benzophenone, arbutin, guaiazulene, shikonin , Baicalin, baicalein, berberine, placenta extract, ellagic acid, rucinol, etc. can be contained.
• vitamin C or its derivative vitamin C phosphate magnesium salt, vitamin C glucoside, etc.
• hydroquinone or its derivative hydroquinone benzyl ether etc.
• kojic acid or its derivative vitamin E or its derivative
• glutathione hydrogen peroxide
• zinc peroxide placenta extract
• ellagic acid arbutin, rucinol
• silk extract botanical extract (camomile, mulberry, gardenia, toucan, weeping locust, Clara, welsh, honeysuckle, Yellowfin moth, matsuhodo, stalk-head moth, oyster spinach, hop, hawthorn, eucalyptus, sturgeon,retea, kishi, mankeissi, hamamelis, karaguwa or yamaguwa, long-lived grass, bellflower, to
• melanin pigment reduction or decomposition substance phenylmercuric hexachlorophene, mercuric oxide, mercuric chloride, hydrogen peroxide water, zinc peroxide, hydroquinone or a derivative thereof can be contained.
• Hydroquinone lactic acid bacteria extract, placenta extract, Ginseng extract, vitamin A, vitamin E, allantoin, spleen extract, thymus extract, yeast extract, fermented milk extract, plant extract (aloe, augon) , Japanese cedar, gentian, burdock, silicon, carrots, hamamelis, hops, yokinin, odrikosou, sageli, toucan, toucan senka, amacha, stinging, cucumber, persimmon, mannen low, parsley) and the like.
• succinic acid As astringents, succinic acid, allantoin, zinc chloride, zinc sulfate, zinc oxide, calamine, zinc paraphenol sulfonate, potassium aluminum sulfate, resorcinol, ferric chloride, tannic acid (including catechin compounds), etc. is there.
• reactive oxygen scavenger SOD, catalase, glutathione peroxidase and the like can be contained.
• beta-carotene As a lipid peroxide formation inhibitor, beta-carotene, plant extract (sesame cultured cells, macula cells, vitiligo, hyperglossia, hamamelis, clove, melissa, emmee, birch, salvia, manen's low, south heaven, agez, ginkgo, green tea) etc can be included It is.
• anti-inflammatory agents ictamol, indomethacin, kaolin, salicylic acid, sodium salicylate, methyl salicylate, acetylsalicylic acid, diphenhydramine hydrochloride, d-camphor, dl-camphor, hydrocortisone, guaiazulene, camazulene, chlorpheniramine maleate, glycyrrhizinic acid or a salt thereof And glycyrrhetinic acid or a salt thereof, licorice extract, shikon extract, Agetsu extract, propolis and the like.
• glycerin As a humectant, glycerin, propylene glycol, 1,3-butylene glycol, polyethylene glycol, glycerin tricaprylic caprate, glycolic acid (alpha-hydroxy acid), hyaluronic acid or a salt thereof, chondroitin sulfate or a salt thereof, water-soluble chitin or a salt thereof Derivative or chitosan derivative, pyrrolidone carboxylic acid or salt thereof, sodium lactate, urea, sorbitol, amino acid or derivative thereof (valine, leucine, isoleucine, threonine, methionine, phenylalanine, tryptophan, lysine, glycine, alanine, asparagine, glutamine, serine, Cysteine, cystine, tyrosine, proline, hydroxyproline, aspartic acid, glutamic acid, hydroxylysine, arginine, orni
• glycolic acid citric acid, malic acid, tartaric acid, lactic acid, ferulic acid, phytic acid and the like can be contained.
• natural animal flavors such as musk, civet, kathrium, ambergris, anise essential oil, angelica essential oil, ylang ylang essential oil, iris essential oil, fennel essential oil, orange essential oil, cananga essential oil, caraway essential oil, cardamom essential oil, guaiac wood essential oil, cumin Essential oil, black letter essential oil, cinnabar essential oil, cinnamone essential oil, geranium essential oil, copaiba balsam essential oil, coriander essential oil, coriander essential oil, shiso essential oil, citronella essential oil, jasmine essential oil, gingergrass essential oil, cedar essential oil, spearmint essential oil, pearl pepper essential oil, large Squid oil essential oil, tuberose essential oil, clove essential oil, orange flower essential oil, winter green essential oil, torubalsam essential oil, batuuri essential oil, rose essential oil, palma rosa essential oil, persimmon essential oil, hiba essential oil, white camellia essential oil
• a capsule containing a spice or the like is embedded in a filter attached to a cigarette or a filter for attaching to a cigarette, a noise, a touch and a smell that a capsule is crushed by a finger can be obtained at the time of smoking.
• a capsule containing a component such as menthol which volatilizes or evaporates or sublimes to improve the passage of the nose
• the capsule can be crushed at the time of nasal congestion to improve nasal congestion.
• a capsule containing a flavor is placed on a grating card, the recipient can squeeze the capsule to obtain sound, feel and smell.
• it can be applied to medical supplies, daily food products such as health food, food, cosmetics, cleaning products and the like.
• Example 1 is a table
• a seamless capsule was manufactured by filling 1-menthol 30% MCT solution into a capsule having a coating ratio of 8.0%, a coating thickness of 25.0 ⁇ m, and a diameter of 4 mm.
• calcium alginate was not treated to replace sodium alginate with calcium alginate.
• the hardness after drying was measured, it was 15N (Kiya-type digital hardness tester KHT-20N type manufactured by Fujiwara Seisakusho Co., Ltd., number of samples: 20).
• KHT-20N type manufactured by Fujiwara Seisakusho Co., Ltd., number of samples: 20.
• the obtained soft capsule was buried in a cigarette filter after drying, it was easily snapped with a finger and cracked, and the sound and feel of cracking of the capsule were enjoyed. I also enjoyed the refreshing scent of menthol.
• the same test is conducted. was gotten.
• a seamless capsule was manufactured by filling 1-menthol 30% MCT solution into a capsule having a coating ratio of 9.0%, a coating thickness of 45.0 ⁇ m, and a diameter of 4 mm.
• a gelatin film when the film ratio was lower than 9.0%, it was difficult to obtain a good capsule.
• the hardness after drying was measured, it was 40N (Kiya-type digital hardness tester KHT-20N type manufactured by Fujiwara Seisakusho Co., Ltd., number of samples: 20).
• Example 2 When the obtained soft capsule composition was embedded in a tobacco filter and sandwiched with fingers in the same manner as in Example 1, it was broken, but it was difficult to be broken, causing pain in the fingers, and the feeling of cracking or sound was not enjoyed. Further, in the same manner as in Example 1, when the tobacco in which the capsule was embedded in the filter was allowed to stand in an environment of 25 ° C. and 85% RH for 10 minutes, the capsule was softened and it became more difficult to break although deformed.
• 1-menthol 30% MCT solution was used to form a seamless capsule having a film rate of 9.0% and a diameter of 4 mm.
• the capsule was broken at the time of drying, and the product could not be manufactured.
• Comparative example 3 When the film ratio was changed to 30% under the same conditions as Comparative Example 2, a seamless capsule having a diameter of 4 mm could be produced.
• the hardness after drying was 40N. However, it was difficult to split by hand.
• Example 2 The capsule obtained in Example 1 was subjected to gelation treatment in an aqueous solution containing calcium ions to improve durability against humidity, and then the immersion treatment time was examined for the redried sample. did.
• Table 4 is a table which shows evaluation of the influence by immersion treatment time.
• the dried capsules are subjected to gelation treatment using a 5% aqueous solution of calcium chloride as a gelling aid aqueous solution, and then the redried samples are stored for a certain time under storage conditions of 40 ° C and 75%.
• Storage the lid of the storage container was in an open state, hereinafter, this is referred to as "capsule release").
• a numerical value such as 1/10 in Table 5 indicates the ratio of the number of capsules that did not snap after storage with a finger.
• As the immersion treatment time as a result of comparing 1 minute, 10 minutes and 60 minutes, 1 minute was optimum. When the immersion time is long, the redrying time is long and the effect of the calcium treatment is also weakened.
• Example 3 Similarly, using the capsule obtained in Example 1, the calcium concentration of the redried sample after gelation treatment in an aqueous solution containing calcium ions to improve durability against humidity It was investigated. Table 5 shows the evaluation of the effect of calcium concentration. The fraction in the lower two rows of the table represents the proportion (NG number / n number) of the samples having a bad collapse method as a result of the test of crushing the capsule with a finger.
• Example 1 After the capsule formation of Example 1 described above, the dried capsule is subjected to gelation treatment for an immersion treatment time of 1 minute using an aqueous solution of calcium chloride and calcium lactate pentahydrate as a gelling aid aqueous solution, and then redried. It was stored (released capsule) for 12.5 hours and 21.5 hours at a storage condition of 25 ° C. and 90%. As a result of comparing 0 (control), 0.2, 0.5, 1, 3, 5% by mass (ratio to external water) as calcium chloride concentration, the one with more than 0% and 1% or less is optimum there were. In addition, the concentration of calcium lactate pentahydrate equivalent to these optimum results was externally attached at 5% by mass.
• Example 4 Similarly, using the capsule obtained in Example 1, after immersion treatment in a calcium-containing ethanol solution to improve durability against humidity, a liquid to be immersed in a sample from which ethanol has been removed
• Tables 7 and 8 show the evaluation of the effects of storage conditions
• Table 7 shows the results of the crushing test with fingers (fractions of the tests for crushing capsules with fingers
• number of NG / number of n is shown.
• the hardness in Table 8 is a unit N, and represents the average value of 10 samples, MAX, MIN, and R, respectively.
• Samples 4A-C are comparative examples. Sample 4A was not treated with calcium, sample 4B was soaked in ethanol containing calcium chloride and lecithin, and sample 4C was soaked in a mixed solution of calcium chloride aqueous solution and ethanol. It is. Sample 4D was subjected to gelation treatment (primary treatment) in an aqueous solution of calcium chloride (0.5 mass% (ratio attached to the solvent)) for 1 minute in immersion treatment time, then subjected to redrying treatment with air, 1 It is the one from which the ethanol on the capsule surface has been removed by immersion (secondary treatment). As a method of removing ethanol, methods such as natural volatilization, volatilization by air blowing, and centrifugation can be used.
• centrifugation is preferably used.
• Samples 4E to K are immersed (1 minute) in a mixture of calcium chloride aqueous solution (0.25, 0.5% by mass) and ethanol (ethanol 30, 50, 60% by mass), and subsequently in ethanol or ethanol After immersion (2 minutes) in a solution in which calcium chloride (0.5 mass%) is dissolved, ethanol on the capsule surface is removed. All were stored at 25 ° C. and 90% high humidity (capsule release).
• samples 4D to K were good. Samples 4D to K were also good in terms of hardness.
• the immersion treatment is carried out with a calcium aqueous solution, re-drying after the treatment is necessary.
• the immersion treatment is carried out with a solution in which calcium is dissolved in ethanol, the effect of the hardening treatment with calcium is diminished. It tended to
• primary immersion treatment is performed with a mixed solution of calcium aqueous solution and ethanol, then secondary immersion treatment is performed with ethanol or ethanol containing calcium chloride, and then capsule surfaces
• the method of removing ethanol is preferred in terms of working efficiency, capsule finish and moisture resistance.
• Example 5 Similarly, in order to improve durability against humidity, alginate was added, gelation was performed in an aqueous solution containing calcium ions, and then in the redried sample, the blending amounts of alginate and plasticizer were examined.
• Table 9 is a table which shows evaluation of the influence by the compounding quantity of an alginate and a plasticizer.
• composition of the capsule shell 1.0 and 5.0 mass% of sodium alginate and 3.0, 6.0 and 10.0 mass% of plasticizer as plasticizer are used.
• the dried capsule is subjected to an immersion treatment using calcium chloride aqueous solution (concentration of calcium chloride as 0.5, 1% by mass (the ratio of external attachment to water)) as an aqueous solution for gelation, and then redried
• the stored sample was stored (released capsule) for 13, 38, 60 and 92 hours under storage conditions of 25 ° C. and 90%.
• the capsule according to the present invention has good storage stability and is easily broken by fingers, it can obtain added value such as sound and feel when broken and can be applied to various uses, so it is practical and industrially useful. high.

Priority Applications (1)

Applications Claiming Priority (4)

Publications (1)

Family

ID=43356176

Family Applications (1)

Country Status (3)

Cited By (15)

Families Citing this family (5)

Citations (9)

Family Cites Families (9)

• 2010
  • 2010-06-16 KR KR1020107015934A patent/KR101038696B1/ko active IP Right Grant
  • 2010-06-16 WO PCT/JP2010/003995 patent/WO2010146845A1/ja active Application Filing
  • 2010-06-16 JP JP2010546567A patent/JP4822299B2/ja active Active
• 2011
  • 2011-09-02 JP JP2011191389A patent/JP5754777B2/ja not_active Ceased
• 2015
  • 2015-05-21 JP JP2015103806A patent/JP2015163716A/ja active Pending
• 2016
  • 2016-08-24 JP JP2016163208A patent/JP6291539B2/ja active Active
• 2018
  • 2018-02-09 JP JP2018021616A patent/JP2018075488A/ja not_active Withdrawn

Patent Citations (11)

Also Published As

Similar Documents

Legal Events