WO2010146845A1 - Soft capsule and manufacturing method therefor - Google Patents
Soft capsule and manufacturing method therefor Download PDFInfo
- Publication number
- WO2010146845A1 WO2010146845A1 PCT/JP2010/003995 JP2010003995W WO2010146845A1 WO 2010146845 A1 WO2010146845 A1 WO 2010146845A1 JP 2010003995 W JP2010003995 W JP 2010003995W WO 2010146845 A1 WO2010146845 A1 WO 2010146845A1
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- WIPO (PCT)
- Prior art keywords
- capsule
- acid
- soft capsule
- carrageenan
- oil
- Prior art date
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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
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- 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.
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Abstract
Description
割れやすくする技術の用途としては、例えば、香料等を内包したカプセルをタバコのフィルターに埋設して、喫煙時などにカプセルを割って香りを楽しんだり、カプセルが割れる際の音や感触を楽しむことなどが挙げられる。しかし、それを好適に実現する従来技術はない。 Soft capsules are widely used in the fields of medicines, cosmetics, health foods and the like. In recent years, 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. However, there is no prior art which suitably realizes it.
しかし、カプセル皮膜を薄くすると硬度は低くなるが、カプセル皮膜自体に相応の可塑性があるため、カプセルは心地よく割れずに変形してしまう。 Generally, in order to make the capsule easy to break, the capsule coating is made thin. For example, 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.
However, although thinning the capsule shell lowers the hardness, the capsule shell deforms comfortably without cracking because the capsule shell itself has adequate plasticity.
例えば皮膜のゲル化剤として、カラギナンを使用することが公知である。しかし、カラギナンは増粘効果が高く、かつ、ゲル化速度も速いので、多量のカラギナンを含有することはカプセル化の妨げになる。すなわち、カラギナンの含有率が高い場合、高粘度と早いゲル化のために、真球性の悪さや射出ノズル先端での固まりやすさなど、カプセルの成形性が悪く、好ましいカプセルが製造できなかった。 In order to avoid the problem, if the content of the gelling agent in the capsule shell is increased, the viscosity becomes high, and the capsule production becomes difficult.
For example, it is known to use carrageenan as a gelling agent for films. However, since 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 .
しかし、吸湿性が高いことが周知であるゼラチンを皮膜に採用した場合は勿論、ゼラチンより吸湿性が低いとされているカラギナンを採用した場合であっても、デンプンや、デキストリン、非ゲル化多糖類などを配合すると、湿度の影響を受けやすくなり、乾燥後における手指での割れやすさ、割れる際の音や感触などの付加価値を、経時的に安定して得ることはできない。 As measures against this, for example, in Patent Document 3, 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.
However, when gelatin is well-known to have high hygroscopicity, of course, 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. When 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.
また、特許文献6には、カラギナンにクエン酸カリウム等を加えることが記載されているが、粘性及び弾性を調整するものとしての開示にとどまっている。
また、特許文献7~14には、タバコのフィルターにカプセルを埋設することが開示されているが、カプセルの製造性や、保存性、乾燥後における手指での割れやすさ、割れる際の音や感触などの付加価値については考慮されていない。 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.
Moreover, although patent document 6 describes adding potassium citrate etc. to carrageenan, it is only indicated as what adjusts viscosity and elasticity.
Further, 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.
例えば、可塑剤は、成形性の向上、アルギン酸塩類は、湿度に対する耐久性の向上に寄与する。なお、アルギン酸塩類は、ただ単に添加するのみでもかまわないが、カルシウムイオンを含む水溶液中でゲル化処理を施してもよい。 Here, the composition of the capsule shell may contain any of a plasticizer, an alginate, a saccharide, a dextrin, a starch, and a processed starch.
For example, plasticizers contribute to the improvement of formability, and 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.
シームレスカプセルは、例えば、従来公知の滴下法によって製造できる。滴下法の典型例は、同心二重ノズルを用いて、外側ノズルからはゲル化剤水溶液等を含む皮膜液を、内側ノズルからは内容物を、各々同時に二重液滴として、皮膜液がゲル化する液の中へ滴下し、外側の皮膜液をゲル化、硬化させてカプセル皮膜とし、継目の無いシームレスカプセルとする製法である。液中硬化法やオリフィス法とも呼ばれることがある。二重ノズルの代わりに三重以上の多重ノズルを用いることも可能である。 As a capsule, it can be usefully applied to a seamless capsule.
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. Sometimes called liquid hardening method or orifice method. Instead of double nozzles, it is also possible to use triple or more multiple nozzles.
本発明者は、ソフトカプセルの製造にあたって、カラギナンを酸で処理することで有用な結果が得られた知見を基に、本発明に至った。 Hereinafter, embodiments of the present invention will be described based on the examples shown in Tables 1 to 8. Note that the embodiment is not limited to the following examples, and design changes can be made as appropriate using conventionally known techniques such as the aforementioned documents without departing from the spirit of the present invention.
The present inventors arrived at the present invention based on the finding that useful results were obtained by treating carrageenan with an acid in the production of soft capsules.
主成分のカラギナンは、κ,ι,λ等のタイプや原料などによって細分類され得るが、基本的にはこれらの内、κタイプが必須であり、ι,λはいずれも適宜利用可能である。
また、例えば日本の食品衛生法では、食品添加物として使用できるカラギナンとして、精製カラギナン・加工ユーケマ藻類・ユーケマ藻類が規定されているが、これらのいずれも使用可能であり、食品添加物としての利用は提供先となる各国の法規による。
従来技術では、ゼラチンを主成分とするものが多いが、カラギナンを主成分とするものには、付着性の低さや、湿度による影響が少ないなどの利点がある。 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 κ, ι, λ, etc. or raw materials, but basically, of these, κ type is essential, and both ι and λ can be appropriately used. .
Further, for example, in the Food Sanitation Law of Japan, 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 Depends on the regulations of each country to which it is provided.
In the prior art, 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.
それに対し、本発明では、無機酸・有機酸のいずれか一方または両方と、各種カチオンを含有させることで、カラギナンに起因する問題点を改善し、しかも、得られたカプセルは、湿度条件によらずに硬さが一定の硬度40N以下であり、手指で簡単に割ることができ、カプセルが割れるときに生じるパチンという音及び感触が心地よいものとなった。また、略球形のシームレスカプセルが得られるので、美観の点でも好ましい成形が容易である。 On the other hand, 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.
On the other hand, in the present invention, 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. In addition, since a substantially spherical seamless capsule can be obtained, preferred molding is easy in view of aesthetics.
このように低い皮膜率であっても、乾燥工程や輸送過程においても、破裂や変形のない良好なカプセルが得られた。
また、製造性や割れやすさなどの点から、カプセル皮膜の硬度は、5~40N、好ましくは10~20N、カプセル皮膜の厚さは、40μm以下、好ましくは30μm以下、掴みやすさや内容量などの点から、カプセルの直径は、0.5~15mm、好ましくは1~8mmであることが好適である。 The content of carrageenan in the composition of the capsule shell is 50% or more, preferably 70% or more. Also, 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.
In addition, 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 μm or less, preferably 30 μm 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.
カラギナンを分解する程度は、カプセルの内容物との兼ね合いなどによって、好ましい粘度までに調整する。 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.
なお、カプセル中に含まれているアルギン酸塩類は、カルシウムイオンを含む水溶液(例:塩化カルシウム水溶液、乳酸カルシウム水溶液など。以下、ゲル化助剤水溶液という。)中でゲル化処理を施してもよい。
アルギン酸カルシウムは、原料としての使用には適さないが、その後のゲル化助剤水溶液中のカルシウムイオンとの反応によって、各種アルギン酸塩類からアルギン酸カルシウムに変化し得るので、最終的なカプセルの中には含まれ得る。ゲル化処理の方法としては、(1)皮膜液調製時にアルギン酸ナトリウムを溶解後にゲル化助剤水溶液を添加する方法、(2)カプセル形成後、乾燥前に(カプセル皮膜に水分が含まれている状態で)ゲル化助剤水溶液に浸漬する方法、(3)カプセル形成後、乾燥したカプセルをゲル化助剤水溶液に浸漬する方法などを例示することができる。
なお、本発明において、アルギン酸塩類は必須成分ではなく、あくまでも吸湿防止目的の任意的添加物である。 Also, in order to improve the resistance to humidity, 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). .
Although 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. As a method of gelation treatment, (1) a method in which an aqueous solution of gelling aid is added after dissolving sodium alginate at the time of preparation of a coating solution, (2) after capsule formation, before drying (the capsule coating contains water In the state, a method of immersing in an aqueous solution of gelation aid, (3) A method of immersing a dried capsule in an aqueous solution of gelation aid, etc. after capsule formation can be exemplified.
In the present invention, alginic acid salt is not an essential component, and is merely an optional additive for the purpose of preventing moisture absorption.
前記(3)の方法で処理する場合の浸漬処理時間に関しては、特に限定されるものではないが、あまり長時間処理を行っても効果が増強されないため、10分以内が好ましく、1~3分程度が最も好ましい。 Although 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.
塩化カルシウム水溶液を用いた場合の最適な水溶液濃度は1質量%以下である。 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.
コーティング方法としては、乾燥後のカプセルに、コーティング剤を揮発性溶媒などに溶解または分散したものを噴霧または塗布し、揮発性溶媒を揮散させる方法(上掛け法)、コーティング剤を揮発性溶媒などに溶解または分散させたものに乾燥後のカプセルを浸漬し、揮発性溶媒を揮散させる方法(ディップ法)、カプセル皮膜液調製時に予め分散・懸濁させておく方法(練り込み法)などを挙げることができ、特にその方法に制限はない。
なお、コーティング剤をカプセル皮膜に導入する場合には、分散性や懸濁性を高めるために、乳化剤を適宜配合してもよい。 Furthermore, in order to enhance the moisture absorption prevention property, coating may be performed with various coating agents such as waxes and waxes described later.
As 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). There is no particular limitation on the method.
When the coating agent is introduced into the capsule shell, an emulsifying agent may be appropriately blended in order to enhance the dispersibility and the suspension.
以下に、カプセルに含有し得るものを例示する。これら各成分は、カプセル剤中のいかなる部分にも含有可能である。 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.
例えば、たばこに付属しているフィルターや、たばこに取り付けるためのフィルターの内部に、香料等を内包したカプセルを埋設すれば、喫煙時に指でつぶしてカプセルがつぶれる音や感触と香りが得られる。また、マスク内に、揮発または蒸発または昇華して、鼻のとおりが良くなるメントール等の成分を内包したカプセルを埋設すれば、鼻づまり時にカプセルをつぶして鼻づまりを改善できる。また、グレーティングカードにフレーバーを内包したカプセルを設置すれば、受取人がカプセルをつぶして音や感触と香りを得られる。
その他、医薬品や、健康食品、食品、化粧品、清掃用品等の日用品などに適用可能である。 Various applications are possible depending on such inclusions.
For example, if 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. In addition, if a capsule containing a component such as menthol which volatilizes or evaporates or sublimes to improve the passage of the nose is embedded in the mask, the capsule can be crushed at the time of nasal congestion to improve nasal congestion. Also, if a capsule containing a flavor is placed on a grating card, the recipient can squeeze the capsule to obtain sound, feel and smell.
In addition, it can be applied to medical supplies, daily food products such as health food, food, cosmetics, cleaning products and the like.
表1は、本発明による実施例のカプセル皮膜の組成を示す表である。 Example 1
Table 1 is a table | surface which shows a composition of the capsule film of the Example by this invention.
乾燥後の硬度を測定すると、15N((株)藤原製作所製 木屋式デジタル硬度計KHT-20N型、サンプル数20)であった。
得られたソフトカプセルを、乾燥後にタバコフィルターに埋設したところ、手指で容易にパチンと音を立てて割れ、カプセルが割れる音と感触を楽しめた。またメントールの爽快な香りも楽しめた。
更に、高湿条件下での安定性のテストとして、カプセルをフィルターに埋設したタバコを、25℃85%RHの環境下に10分間放置後、同様のテストをしたところ、前記とほぼ同様の結果が得られた。 As a capsule content, 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 μm, and a diameter of 4 mm. However, in this example, calcium alginate was not treated to replace sodium alginate with calcium alginate.
When 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).
When 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.
Furthermore, as a test of stability under high humidity conditions, when a cigarette in which the capsule is embedded in a filter is left in an environment of 25 ° C. and 85% RH for 10 minutes, the same test is conducted. was gotten.
表2は、比較例1のカプセル皮膜の組成を示す表である。 (Comparative example 1)
Table 2 is a table showing the composition of the capsule film of Comparative Example 1.
乾燥後の硬度を測定すると、40N((株)藤原製作所製 木屋式デジタル硬度計KHT-20N型、サンプル数20)であった。
得られたソフトカプセル組成物を、実施例1と同様にタバコフィルターに埋設し手指で挟んだところ、割れたが、割れにくく、指に痛みを生じ、割れる感触や音は楽しめなかった。
また、実施例1と同様に、カプセルをフィルターに埋設したタバコを、25℃85%RHの環境下に10分間放置したところ、カプセルが軟化して、変形はするものの一層割れにくくなった。 As a capsule content, 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 μm, and a diameter of 4 mm. In the case of a gelatin film, when the film ratio was lower than 9.0%, it was difficult to obtain a good capsule.
When 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).
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.
表3は、比較例2のカプセル皮膜の組成を示す表である。 (Comparative example 2)
Table 3 shows the composition of the capsule film of Comparative Example 2.
しかし、乾燥時にカプセルが割れてしまい、製品は製造できなかった。 As a capsule content, 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.
However, the capsule was broken at the time of drying, and the product could not be manufactured.
比較例2と同様の条件で、皮膜率を30%に変えたところ、直径4mmのシームレスカプセルを製造できた。乾燥後の硬度は40Nであった。
しかし、手指で割ることは困難であった。 (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.
比較例2と同様の条件で、皮膜率を20%に変えたところ、直径4mmのシームレスカプセルを成形できた。
しかし、乾燥時に2割程のカプセルが割れてしまい、収率が悪く、安定した製造はできなかった。また、デキストリンの吸湿性に起因して、形状がいびつで、球状のカプセルは製造できなかった。
数少ない良品を選別して試験に供したところ、製造品の乾燥後の硬度は25Nであった。手指で割ると、割れたが、割れにくく、指に痛みを生じた。また、25℃85%RHの環境下に10分間放置したところ、カプセルは皺だらけになると共に軟化し、押してもプスッとつぶれるだけであった。 (Comparative example 4)
When the film ratio was changed to 20% under the same conditions as Comparative Example 2, a seamless capsule having a diameter of 4 mm could be formed.
However, about 20% of the capsules were broken at the time of drying, the yield was poor, and stable production could not be performed. Also, due to the hygroscopicity of dextrin, irregularly shaped spherical capsules could not be produced.
A few non-defective items were selected and tested, and the hardness after drying of the manufactured product was 25 N. I broke it with my fingers, but it was hard to break and I had pain in my fingers. In addition, when left in an environment of 25 ° C. and 85% RH for 10 minutes, the capsule was covered with wrinkles and softened, and was only crushed when pressed.
前記実施例1で得られたカプセルを使用して、湿度に対する耐久性を向上させるためにカルシウムイオンを含む水溶液中でゲル化処理を施した後、再乾燥したサンプルにおいて、その浸漬処理時間を検討した。
表4は、浸漬処理時間による影響の評価を示す表である。 (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.
浸漬処理時間として、1分、10分、60分を比較した結果、1分のものが最適であった。浸漬時間が長時間になると、再乾燥時間が長時間化し、カルシウム処理の効果も薄れていく結果となった。 After forming the capsules of the previous example 1, 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.
同様に、前記実施例1で得られたカプセルを使用して、湿度に対する耐久性を向上させるためにカルシウムイオンを含む水溶液中でゲル化処理を施した後、再乾燥したサンプルにおいて、そのカルシウム濃度を検討した。
表5は、カルシウム濃度による影響の評価を示す表である。なお、表の下部2行における分数は、手指によりカプセルをつぶす試験の結果、不良なつぶれ方をしたサンプルの割合(NG数/n数)を表す。 (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.
塩化カルシウムの濃度として、0(対照)、0.2、0.5、1、3、5質量%(水に対する外付け割合)を比較した結果、0%を超え1%以下のものが最適であった。また、これらの最適な結果と同等な乳酸カルシウム五水和物の濃度は、5質量%外付けのものであった。 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.
同様に、前記実施例1で得られたカプセルを使用して、湿度に対する耐久性を向上させるためにカルシウムを含むエタノール溶液中に浸漬処理を施した後、エタノールを除去したサンプルにおいて、浸漬させる液の組成の差などによる効果の差を検討した。
表6は、処理条件を示す表であり、表7及び8は、保存条件による影響の評価を示す表であり、表7は手指によりつぶす試験の結果(分数は、手指によりカプセルをつぶす試験の結果、不良なつぶれ方をしたサンプルの割合(NG数/n数)を表す。)、表8は硬度を表す。なお、表8における硬度は、単位Nであり、サンプル数10の平均値、MAX、MIN、Rをそれぞれ表す。 (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 We examined the difference of the effect due to the difference of the composition of
Table 6 shows the processing conditions, Tables 7 and 8 show the evaluation of the effects of storage conditions, and Table 7 shows the results of the crushing test with fingers (fractions of the tests for crushing capsules with fingers As a result, the proportion of the sample which smashed in a bad manner (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.
サンプル4Dは、塩化カルシウム水溶液(0.5質量%(溶媒に対する外付け割合))に浸漬処理時間1分でゲル化処理(一次処理)した後、送風による再乾燥処理を行い、エタノール中に1分浸漬(二次処理)し、カプセル表面のエタノールを除去したものである。エタノールの除去の方法としては、自然揮発、送風による揮発、遠心分離などの方法が利用できる。工業的には、遠心分離が好ましく使用される。
サンプル4E~Kは、塩化カルシウム水溶液(0.25、0.5質量%)とエタノールとの混液(エタノール30、50、60質量%)に浸漬(1分)し、続けてエタノールまたはエタノール中に塩化カルシウム(0.5質量%)を溶解した液に浸漬(2分)した後、カプセル表面のエタノールを除去したものである。
いずれも、25℃90%の高湿度条件で保存(カプセル開放)した。 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. Industrially, 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).
カルシウム水溶液で浸漬処理を行った場合には、処理後の再乾燥が必要であり、一方、エタノール中にカルシウムを溶かした液で浸漬処理を行った場合には、カルシウムによる硬化処理の効果が薄れてしまう傾向があった。それに対し、本実施例の特にサンプル4E~Kのように、カルシウム水溶液とエタノールの混液で一次浸漬処理を行い、その後、エタノールまたは塩化カルシウム入りエタノールで二次浸漬処理を行い、次いで、カプセル表面のエタノールを除去する方法は、作業効率と、カプセルの仕上がり及び耐湿性の点で好ましい。 As a result of the finger crushing test, samples 4D to K were good. Samples 4D to K were also good in terms of hardness.
When the immersion treatment is carried out with a calcium aqueous solution, re-drying after the treatment is necessary. On the other hand, when 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 On the other hand, as in the case of samples 4E to K of this example in particular, 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.
同様に、湿度に対する耐久性を向上させるためにアルギン酸塩類を加え、カルシウムイオンを含む水溶液中でゲル化処理を施した後、再乾燥したサンプルにおいて、アルギン酸塩類と可塑剤の配合量を検討した。
表9は、アルギン酸塩類と可塑剤の配合量による影響の評価を示す表である。 (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.
その結果、アルギン酸ナトリウムの配合量による差も、可塑剤のグリセリンの配合量による差も認められなかった。 In the 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. After capsule formation, 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%.
As a result, neither the difference by the compounding quantity of sodium alginate nor the difference by the compounding quantity of the glycerol of a plasticizer was recognized.
Claims (14)
- ソフトカプセルにおいて、そのカプセル皮膜の組成物に、カラギナンと、酸性pH調整剤、中和剤とを少なくとも有することを特徴とするソフトカプセル。 A soft capsule comprising at least a carrageenan, an acidic pH adjuster, and a neutralizing agent in the composition of the capsule shell.
- カプセル皮膜の組成物に、可塑剤、アルギン酸塩類、糖類、デキストリン類、でん粉、加工でん粉の少なくともいずれかを有する請求項1に記載のソフトカプセル。 The soft capsule according to claim 1, wherein the composition of the capsule shell comprises at least one of a plasticizer, an alginate, a saccharide, a dextrin, a starch, and a processed starch.
- カラギナンが、酸性pH調整剤による分解で粘度の調整されたものである請求項1または2に記載のソフトカプセル。 The soft capsule according to claim 1 or 2, wherein carrageenan is one whose viscosity is adjusted by decomposition with an acidic pH adjuster.
- カプセル皮膜の組成物におけるカラギナンの含有率が、50%以上、好ましくは70%以上である請求項1ないし3のいずれかに記載のソフトカプセル。 4. The soft capsule according to any one of claims 1 to 3, wherein the content of carrageenan in the composition of the capsule shell is 50% or more, preferably 70% or more.
- 皮膜率が、5~20%、好ましくは7~15%である請求項1ないし4のいずれかに記載のソフトカプセル。 The soft capsule according to any one of claims 1 to 4, wherein the coating rate is 5 to 20%, preferably 7 to 15%.
- カプセル皮膜の厚さが、40μm以下、好ましくは30μm以下である請求項1ないし5のいずれかに記載のソフトカプセル。 The soft capsule according to any one of claims 1 to 5, wherein the thickness of the capsule shell is 40 μm or less, preferably 30 μm or less.
- カプセル皮膜の硬度が、5~40N、好ましくは10~20Nである請求項1ないし6のいずれかに記載のソフトカプセル。 The soft capsule according to any one of claims 1 to 6, wherein the hardness of the capsule shell is 5 to 40N, preferably 10 to 20N.
- カプセルの直径が0.5~15mm、好ましくは1~8mmである請求項1ないし7のいずれかに記載のソフトカプセル。 Soft capsule according to any of the preceding claims, wherein the capsule diameter is 0.5-15 mm, preferably 1-8 mm.
- カプセルがシームレスカプセルである請求項1ないし8のいずれかに記載のソフトカプセル。 The soft capsule according to any one of claims 1 to 8, wherein the capsule is a seamless capsule.
- アルギン酸塩類の含有率が、カラギナンの50%以下である請求項2ないし9のいずれかに記載のソフトカプセル。 The soft capsule according to any one of claims 2 to 9, wherein the content of alginate is 50% or less of that of carrageenan.
- ロウ類、ワックス類または硬化油から選ばれる一種以上から成るコーティングを有する請求項1ないし10のいずれかに記載のソフトカプセル。 The soft capsule according to any one of claims 1 to 10, having a coating comprising one or more selected from waxes, waxes or hydrogenated oils.
- ソフトカプセルの皮膜を調製する方法において、カプセル皮膜の組成物となるカラギナンを酸性pH調整剤によって分解する工程と、その分解を中和剤によって停止する工程とを備えることを特徴とするソフトカプセルの製造方法。 A method of producing a soft capsule, comprising the steps of: decomposing carrageenan, which is a composition of the capsule coating, with an acidic pH adjuster; and stopping the degradation with a neutralizing agent. .
- カプセル皮膜の組成物としてアルギン酸塩類を加え、アルギン酸塩類は、カルシウムイオンを含むゲル化助剤水溶液中でゲル化処理する請求項12に記載のソフトカプセルの製造方法。 The method for producing a soft capsule according to claim 12, wherein an alginate is added as a composition of the capsule shell, and the alginate is subjected to a gelling treatment in an aqueous solution of a gelling aid containing calcium ions.
- ゲル化助剤水溶液に、エタノールを含有させて用いる請求項12または13に記載のソフトカプセルの製造方法。 The method for producing a soft capsule according to claim 12 or 13, wherein the aqueous solution of gelation aid contains ethanol.
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Also Published As
Publication number | Publication date |
---|---|
JP6291539B2 (en) | 2018-03-14 |
JP2017039724A (en) | 2017-02-23 |
JP2015163716A (en) | 2015-09-10 |
JPWO2010146845A1 (en) | 2012-11-29 |
KR20110007081A (en) | 2011-01-21 |
JP4822299B2 (en) | 2011-11-24 |
KR101038696B1 (en) | 2011-06-02 |
JP2012001553A (en) | 2012-01-05 |
JP5754777B2 (en) | 2015-07-29 |
JP2018075488A (en) | 2018-05-17 |
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