Source: http://www.google.com/patents/US5478508?dq=6,654,957
Timestamp: 2017-06-26 02:44:17
Document Index: 317534654

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Patent US5478508 - Method of producing seamless capsule - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsA process for producing a seamless capsule wherein a two-layer droplet is ejected from a double orifice type nozzle in an aqueous hardening liquid, and an outer layer of the droplet is hardened under cooling, the viscosity of the aqueous hardening liquid being made within the range of 20 to 100 mPa·s,...http://www.google.com/patents/US5478508?utm_source=gb-gplus-sharePatent US5478508 - Method of producing seamless capsuleAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS5478508 APublication typeGrantApplication numberUS 08/143,475Publication dateDec 26, 1995Filing dateOct 26, 1993Priority dateOct 28, 1992Fee statusLapsedAlso published asDE69307264D1, DE69307264T2, EP0595263A1, EP0595263B1Publication number08143475, 143475, US 5478508 A, US 5478508A, US-A-5478508, US5478508 A, US5478508AInventorsToshiyuki Suzuki, Masayuki Ikeda, Takahiro OkudaOriginal AssigneeFreund Industrial Co., Ltd.Export CitationBiBTeX, EndNote, RefManPatent Citations (15), Referenced by (35), Classifications (16), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetMethod of producing seamless capsule
A process for producing a seamless capsule wherein a two-layer droplet is ejected from a double orifice type nozzle in an aqueous hardening liquid, and an outer layer of the droplet is hardened under cooling, the viscosity of the aqueous hardening liquid being made within the range of 20 to 100 mPa·s, and any difference in specific gravity between any two of the liquids of the layers ejected from the nozzle and the aqueous hardening liquid is made within 0.05.
1. A method of producing a seamless capsule, wherein, a two-layer droplet is ejected from a double orifice type nozzle into an aqueous hardening liquid, and an outer layer of the droplet is hardened under cooling, characterized in that a viscosity of said aqueous hardening liquid is within a range of 20 to 100 mPa·s.
5. A method of producing a seamless capsule, wherein a two-layer droplet is ejected from a double orifice type nozzle into an aqueous hardening liquid, and an outer layer of the droplet is hardened under cooling, characterized in that viscosity of the aqueous hardening liquid is within a range of 20 to 100 mPa·s and a difference in specific gravity between any two of liquids of layers ejected from the double orifice of the nozzle and the aqueous hardening liquid is within 0.05.
In principle, it is advantageous to constitute an outer layer by a lipophilic substance in order to produce a seamless capsule which seals water and can be preserved for a long time. Thus, the present inventors have intensively studied this type of constitution to find that for achieving above purposes, it is effective to satisfy either a condition that the viscosity of the hardening liquid is within 20 to 100 mPa·s or a condition that difference of the specific gravities between any two of three solutions, i.e., the core solution, the solution for an outer layer and the hardening liquid, is within 0.05, and when both the conditions are satisfied, more excellent results can be obtained, whereby accomplishing the present invention.
In one embodiment of the invention, the viscosity of the aqueous hardening liquid is set within 20 to 100 mPa·s.
According to the investigation by the present inventors, if the viscosity of the aqueous hardening liquid is less than 20 mPa·s, a jet stream ejected from the orifice becomes unstable and oscillates irregularly, and thus, the size of the droplets varies in wide range or unevenness in wall thickness or eccentricity of the outer layer occurs. On the other hand, if it exceeds 100 mPa·s, it was found that resistance to the jet stream becomes large and its flow rate can not be set to a value suitable for practical production rate.
TABLE 1__________________________________________________________________________Embodiment 1                   Flow rate or SpecificComposition             Flow speed                          Viscosity                                gravity                                     Temperature__________________________________________________________________________Core liquid Purified water:              100 parts                   0.22 ml/sec                          --    1.000                                     22.6° C.Outer layer Fatty acid ester of glycerin               70 parts                   0.10 ml/sec                          --    0.943                                     70.0° C.solution (melting point 42° C.): Fatty acid ester of sucrose               30 parts (melting point 36° C.):Hardening Purified water:               99 parts                   9 cm/sec                          60 mPa · s                                1.005                                     32.0° C.soution HPC-H:*       1 parts__________________________________________________________________________ *Nippon Soda Co. Ltd., see catalog for NISSO HYDROXY PROPYL CELLULOSE, also mentioned in the Pharmacopeia of Japan.
TABLE 2__________________________________________________________________________Embodiment 2                   Flow rate or SpecificComposition             Flow speed                          Viscosity                                gravity                                     Temperature__________________________________________________________________________Core liquid Purified water:              100 parts                   0.22 ml/sec                          --    1.000                                     22.6° C.Outer layer Fatty acid ester of glycerin               50 parts                   0.10 ml/sec                          --    0.980                                     70.0° C.solution (melting point 42° C.): Fatty acid ester of sucrose               50 parts (melting point 36° C.):Hardening Purified water:               99.75                   9 cm/sec                          6 mPa · s                                1.002                                     32.0° C.              partssoution HPC-H:*       0.25              parts__________________________________________________________________________ *Nippon Soda Co. Ltd., see catalog for NISSO HYDROXY PROPYL CELLULOSE, also mentioned in the Pharmacopeia of Japan.
TABLE 3__________________________________________________________________________Embodiment 3                   Flow rate or SpecificComposition             Flow speed                          Viscosity                                gravity                                     Temperature__________________________________________________________________________Core liquid Purified water:              100 parts                   0.22 ml/sec                          --    1.000                                     22.6° C.Outer layer Fatty acid ester of glycerin               50 parts                   0.10 ml/sec                          --    0.980                                     70.0° C.solution (melting point 42° C.): Fatty acid ester of sucrose               50 parts (melting point 36° C.):Hardening Purified water:               99 parts                   9 cm/sec                          6 mPa · s                                1.005                                     32.0° C.soution HPC-H:*       1 parts__________________________________________________________________________ *Nippon Soda Co. Ltd., see catalog for NISSO HYDROXY PROPYL CELLULOSE, also mentioned in the Pharmacopeia of Japan.
TABLE 4__________________________________________________________________________Comparative example                   Flow rate or SpecificComposition             Flow speed                          Viscosity                                gravity                                     Temperature__________________________________________________________________________Core liquid Purified water:              100 parts                   0.22 ml/sec                          --    1.000                                     22.6° C.Outer layer Fatty acid ester of glycerin               70 parts                   0.10 ml/sec                          --    0.943                                     70.0° C.solution (melting point 42° C.): Fatty acid ester of sucrose               30 parts (melting point 36° C.):Hardening Purified water:               99.75                   9 cm/sec                          6 mPa · s                                1.002                                     32.0° C.              partssoution HPC-H:*       0.25              parts__________________________________________________________________________ *Nippon Soda Co. Ltd., see catalog for NISSO HYDROXY PROPYL CELLULOSE, also mentioned in the Pharmacopeia of Japan.
TABLE 6__________________________________________________________________________Embodiment 4                   Flow rate or SpecificComposition             Flow speed                          Viscosity                                gravity                                     Temperature__________________________________________________________________________Core liquid Plum liqueur:              100 parts                   1.38 ml/sec                          --    1.028                                     25.0° C.Outer layer Fatty acid ester of glycerin               50 parts                   0.59 ml/sec                          --    0.980                                     70.0° C.solution (melting point 42° C.): Fatty acid ester of sucrose               50 parts (melting point 36° C.):Hardening Purified water:               99 parts                   9 cm/sec                          60 mPa · s                                1.005                                     23.0° C.soution HPC-H:        1 parts__________________________________________________________________________
TABLE 7__________________________________________________________________________Embodiment 5                   Flow rate or SpecificComposition             Flow speed                          Viscosity                                gravity                                     Temperature__________________________________________________________________________Core liquid Bupleurem Root    0.11 ml/sec                          --    1.029                                     40.7° C. extract:     125 parts Purified water:               75 partsOuter layer Fatty acid ester of glycerin               50 parts                   0.10 ml/sec                          --    0.980                                     70.0° C.solution (melting point 42° C.): Fatty acid ester of sucrose               50 parts (melting point 36° C.):Hardening Purified water:               99 parts                   9 cm/sec                          60 mPa · s                                1.005                                     32.0° C.soution HPC-H:        1 parts__________________________________________________________________________
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in ternary nozzle with atomiser air-dispersing core and wall substancesFR2336176A1 * Title not availableJPH0352639A * Title not availableJPS5689833A * Title not available* Cited by examinerReferenced byCiting PatentFiling datePublication dateApplicantTitleUS5882680 *Dec 3, 1996Mar 16, 1999Freund Industrial Co., Ltd.Seamless capsule and method of manufacturing the sameUS5939097 *Aug 4, 1994Aug 17, 1999Freund Industrial Co., Ltd.Food-like medicineUS6048562 *Jun 28, 1996Apr 11, 2000Nestec S.A.Encapsulation processUS6780507 *Feb 9, 2001Aug 24, 2004Analytical Research Systems, Inc.Hydrocapsules and method of preparation thereofUS8070466 *Sep 25, 2007Dec 6, 2011Freund CorporationSeamless capsule manufacturing apparatusUS8535713Apr 4, 2008Sep 17, 2013Sigmoid Pharma LimitedPharmaceutical cyclosporin compositionsUS8911777Apr 4, 2008Dec 16, 2014Sigmoid Pharma LimitedPharmaceutical composition of tacrolimusUS8951570Apr 25, 2008Feb 10, 2015Sigmoid Pharma LimitedManufacture of multiple minicapsulesUS9114071Apr 4, 2008Aug 25, 2015Sigmoid Pharma LimitedOral pharmaceutical compositionUS9220681Jul 5, 2013Dec 29, 2015Sigmoid Pharma LimitedFormulationsUS9259030Mar 25, 2011Feb 16, 2016Philip Morris Usa Inc.Fabrication of core/shell capsules of different geometries and treatment thereafterUS9278070May 18, 2010Mar 8, 2016Sigmoid Pharma LimitedComposition comprising oil dropsUS9387179Jul 15, 2013Jul 12, 2016Sigmoid Pharma LimitedPharmaceutical cyclosporin compositionsUS9402788Dec 30, 2014Aug 2, 2016Sigmoid Pharma LimitedManufacture of multiple minicapsulesUS9585844Jun 29, 2015Mar 7, 2017Sigmoid Pharma LimitedOral pharmaceutical compositionUS20020050659 *Feb 9, 2001May 2, 2002William TorekiHydrocapsules and method of preparation thereofUS20040159241 *Feb 18, 2003Aug 19, 2004Bailey Bradley LeeAlcoholic beverage deviceUS20060018965 *Sep 28, 2005Jan 26, 2006Joey MoodleySolid oral dosage form containing seamless microcapsulesUS20070292523 *Sep 27, 2005Dec 20, 2007Joey MoodleyDihydropyrimidine FormulationsUS20080020018 *Sep 27, 2005Jan 24, 2008Joey MoodleyCombination ProductsUS20080113031 *Sep 27, 2005May 15, 2008Joey MoodleyMinicapsule FormulationsUS20080286408 *Dec 11, 2007Nov 20, 2008Philip Morris Usa Inc.Encapsulation of a hydrophilic substance in small capsulesUS20090004337 *May 29, 2008Jan 1, 2009Philip Morris Usa Inc.Wax capsules containing hydrophilic coresUS20100040717 *Sep 25, 2007Feb 18, 2010Narimichi TakeiSeamless capsule manufacturing apparatusUS20100203120 *Apr 4, 2008Aug 12, 2010Ivan CoulterPharmaceutical cyclosporin compositionsUS20100239665 *May 1, 2008Sep 23, 2010Ivan CoulterPharmaceutical nimodipine compositionsUS20100255087 *Apr 4, 2008Oct 7, 2010Ivan Coulteroral pharmaceutical compositionUS20100297221 *Apr 4, 2008Nov 25, 2010Ivan Coulterpharmaceutical composition of tacrolimusUS20110052645 *Apr 25, 2008Mar 3, 2011Ivan CoulterManufacture of multiple minicapsulesEP2322146A2Sep 27, 2005May 18, 2011Sigmoid Pharma LimitedMicrocapsule formulations comprising two pharmaceutically active ingredientsEP2359817A2Mar 29, 2004Aug 24, 2011Sigmoid Pharma LimitedSolid oral dosage form containing seamless microcapsulesEP2444071A1Sep 27, 2005Apr 25, 2012Sigmoid Pharma LimitedMinicapsule formulationsWO2004084870A1Mar 29, 2004Oct 7, 2004Sigmoid Biotechnologies LimitedSolid oral dosage form containing seamless microcapsulesWO2007103557A2Mar 9, 2007Sep 13, 2007Reliant Pharmaceuticals, Inc.Coating capsules with active pharmaceutical ingredientsWO2016044805A1Sep 18, 2015Mar 24, 2016Virun, Inc.Soft gel compositions and pre-gel concentrates* Cited by examinerClassifications U.S. Classification264/4, 424/451, 426/102, 426/96, 426/592, 264/4.3, 264/4.4International ClassificationA61J3/07, B01J13/04, B01J13/14Cooperative ClassificationA61K9/5089, A61K9/4833, B01J13/04European ClassificationA61K9/48C, A61K9/50P, B01J13/04Legal EventsDateCodeEventDescriptionOct 26, 1993ASAssignmentOwner name: FREUND INDUSTRIAL CO., LTD., JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:SUZUKI, TOSHIYUKI;IKEDA, MASAYUKI;OKUDA, TAKAYIRO;REEL/FRAME:006745/0652Effective date: 19931019Jul 20, 1999REMIMaintenance fee reminder mailedDec 26, 1999LAPSLapse for failure to pay maintenance feesMar 7, 2000FPExpired due to failure to pay maintenance feeEffective date: 19991226RotateOriginal ImageGoogle Home - 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