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US2809918A - Sustained release pharmaceutical preparations - Google Patents

Sustained release pharmaceutical preparations
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US2809918A
US2809918AUS541032AUS54103255AUS2809918AUS 2809918 AUS2809918 AUS 2809918AUS 541032 AUS541032 AUS 541032AUS 54103255 AUS54103255 AUS 54103255AUS 2809918 AUS2809918 AUS 2809918A
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crushing
granular
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drying
mixing
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Victor M Hermelin
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United, StatesPatent RELEASE PHARMACEUTICAL PREPARATIONS Victor M. Hermelin, University City, Mo.
Application October 17, 1955, Serial No. 541,032
11 Claims. Cl. 167-82) U A NE N Drawing.
This invention relates in general to certain new and useful improvements in pharmaceutical preparations and, more'particularly, to a unique type of enteric coated beadlet containing a drug or medicament.
The medical'profession frequently has need for drugs or medicaments which can be administered to the patient for purposes of achieving a very quick pharmacological therapeutic efrectand will also maintain such effect over a prolonged period of time. Unfortunately, many drugs and particularly sedatives and hypnotics usually produce a sedated or narcotized condition of relatively short duration and are administered in comparatively light doses in order toavoid toxic reactions or other side efiects which would be harmful to the patient. Similarly, there are some syndromes which may call for administration of a drug which should enter the patients system in small doses at spaced intervals.
It is the primary object of the present invention, therefore, to provide a type of pharmaceuticalpreparation which is capable of producing both a quick initial effect and repetitive effect at spaced intervals over any desired or predetermined period of time.
It is another object of the present invention to provide a pharmaceutical preparation having the combined effects of prompt initial action and prolonged repetitive effect, which preparation is simple to administer, is relatively economical in cost of manufacture, and provides the physician with a very flexible type of materia medica from which to Prescribe.
With'theabove and other objects in view, myinven tion residesin the novel features of form, construction, arrangement, and combination ofparts presently described and pointed out in the claims.
' Broadly speaking, the present invention resides in the discovery, that it is possible to form a beadlet having a more or less spherical inactive core around which successivelayers of the drug or medicament are built up, such layers being separated by enteric envelope-layers formedofa mixture of shellac and stearic, acid. The
enteric coatings or enveloping layers will resist the action of the fluids inthe stomach and intestines for a predeterminedfperiod of time. The outer envelope containing the initial dosei s preferably coated or encased in the usual readily soluble sugar coating capable of being dissolved in the stomach juices.
The follow ng procedure, is illustrative oithe present invention: 7 H H 20 lbs. screened cane sugar in coating pan 20 oz. colored simple syrup added Pan rotated until mixed thoroughly 1 scoop 1b.) powderedsugar and talc added 2 varying from 25 minutes to minutes. An extra half hour of drying time added at end of run to assure all beads being dry. Screened through 10 on 20 and mesh screens. Yield:
/2"lb. on 10 mesh (tailings, agglomerates) 28 lbs. on 20 mesh 11 lbsLon 40 mesh 1 lb. through 40mesh (fines) 41 lbs.
It will, of course, be understood that the above quantities are merely illustrative of the method by which the inactive cores are formed. It also should be pointed out that for any particular batch one size of bead should be used and, the other sizes, which are screened out, should be used for other purposes or for other batches.
Thereupon, a' weighed quantity of slow-release granules made in accordance with the procedure described in my copending application Serial No. 541,027, filed contemporaneously herewith, are crushed finely, but not pulverized. Then, a weighed quantity of the inactive beads or cores are placed in a coating pan and the pan set in motion. A quantity of. the shellac (3 lb. cut U. S. P. grade) is then poured into the pan sulficicnt to thoroughly wet the surfaces of the beads and, thereupon, a quantity of the crushed granules is introduced slowly into the pan until the wet surfaces of the beadlets are dried up. Then, more of the shellac is added and again crushed granules are introduced until a second substantially dry coating has been formed. This procedure is repeated until the desired amount of crushed granules have been applied tothe cores to form a mass of discrete beadlets.
If desired, the beadlets can be trimmed up by applying a conventional outer coating of colored sugar glaze. The above-described procedure can be applied in compounding any of the drugs or medicaments mentioned in the aboveridentified copending application.
It should be understood that changes and modifications in the form, construction, arrangement, and combination of-the several parts ofthe pharmaceutical preparation may be made and substituted for those herein shown and described without departing from the nature and principle of my invention.
Having thus described my invention, what. I claim and desire to secure by Letters Patent is:
1. The process formaking sustained period minuteincremental dosage pharmaceutical preparations which comprises intimately mixing'a powdered'drug and an 1 enteric Water insoluble excipient to produce a pasty Air blown into coating pan during rotation cycle of about one-half hour. Repeated 9. times, amounts of syrup varying from 20 oz.-.to. 32 oz; and amounts, of powdered sugar and talc (10% varying fromJ/z lb. to l lb. at each application, depending on conditions. Time intervals (drying) mass, drying the mass slowly without agitation in such a manner as to produce a rough granular material, breaking up the rough granular material by light crushing, whereby to reduce it to granular particles, said mixing, drying and crushing operations constituting one cycle, and remixing the granular particles with an additional quantity of the excipient to produce a pasty mass, redrying such pasty mass slowly and without agitation in such a manner asto produce a granular material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process consisting of not less than three nor more than fifteen mixing-crushing and drying cycles repeated in successive order whereby toproduce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubilityin the gastro-intestinal tract, lightly crushing said finished granules to form a granular powder, forming a'plurality of ginert seed-like cores, placing said cores in a coating pan; rotating the coating pan, introducing thereinto a water insoluble excipient, dusting in said granular powder, and continuing the addition of water insoluble excipient and granular powder until the desired dosage has been incorporated in the batch.
2. The process for making sustained period minute-inc'remental dosage pharmaceutical preparations which comprises intimately mixing a powdered drug and shellac to produce a pasty mass, drying the mass slowly without agitation in such a manner as to produce a rough granular material, breaking up the rough granular material by light crushing, whereby to reduce it to granular particles, said mixing, drying and crushing operations constituting one cycle, and remixing the granular particles with an additional quantity of shellac to produce a pasty mass, redrying such pasty mass slowly and with out agitation in such a manner as to produce a granular material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process consisting of not less than three nor more than fifteen mixing, crushing and drying cycles repeated in successive order whereby to produce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubility in the gastrointestinal tract, lightly crushing said finished granules to form a granular powder, forming a plurality of inert seed-like cores, placing said cores in a coating pan, rotating the coating pan, introducing thereinto shellac, dusting in said granular powder, and continuing the addition of shellac and granular powder until the desired dosage has been incorporated in the batch.
3. The process for making sustained period minuteincremental dosage pharmaceutical preparations which comprises intimately mixing a powdered drug and an enteric water insoluble excipient consisting of a mixture of shellac and stearic acid, whereby to produce a pasty mass, drying the mass slowly without agitation in such a manner as to produce a rough granular material, breaking up the rough granular material by light crushing, whereby to reduce it to granular particles, said mixing, drying and crushing operations constituting one cycle, and remixing the granular particles with an additional quantity of the excipient to produce a pasty mass, redrying such pasty mass slowly and without agitation in such a manner as to produce a granular material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process consisting of not less than three nor more than fifteen mixing, crushing and drying cycles repeated in successive order whereby to produce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubility in the gastro-intestinal tract, lightly crushing said finished granules to form a granular powder, forming a plurality of inert seed-like cores, placing said cores in a coating pan, rotating the coating pan, introducing thereinto a water insoluble excipient, dusting in said granular powder, and continuing the addition of water insoluble excipient and granular powder until the desired dosage has been incorporated in the batch.
4. The process for making sustained period minuteincremental dosage pharmaceutical preparations which comprises intimately mixing a powdered drug and an enteric water insoluble excipient to produce a pasty mass, placing the mass on trays and drying the mass slowly without agitation in such a manner as to produce a rough granular material, breaking up the rough granular material by light crushing, whereby to reduce it to granular particles, said mixing, drying and crushing operations constituting one cycle, and remixing the granular particles with an additional quantity of the excipient to produce a pasty mass, redrying such pasty mass slowly and without agitation in such a manner as to produce a granular material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process consisting of not less than three nor more than fifteen mixing, crushing and drying cycles repeated in successive order whereby to produce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubility in the gastrointestinal tract, lightly crushing said finished granules to form a granular powder, forming a plurality of inert seed-like cores, placing said cores in a coating pan, rotating the coating pan, introducing thereinto a water insoluble excipient, dusting in said granular powder, and continuing the addition of water insoluble excipient and granular powder until the desired dosage has been incorporated in the batch.
5. The process for making sustained period minuteincremental dosage pharmaceutical preparations which comprises intimately mixing a powdered drug and an enteric water insoluble excipient to produce a pasty mass, spreading the mass in a thin layer upon trays and drying the mass slowly without agitation in such a manner as to produce a rough granular material, breaking up the rough granular material by light crushing, whereby to reduce it to granular particles, said mixing, drying and crushing operations constituting one cycle, and remixing the granular particles with an additional quantity of the excipient to produce a pasty mass, redrying such pasty mass slowly and without agitation in such a manner as to produce a granular material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process consisting of not less than three nor more than fifteen mixing, crushing and drying cycles repeated in successive order whereby to produce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubility in the gastro-intestinal tract, lightly crushing said finished granules to form a granular powder, forming a plurality of inert seed-like cores, placing said cores in a coating pan, rotating the coating pan, introducing thereinto a water insoluble excipient, dusting in said granular powder, and continuing the addition of water insoluble excipient and granular powder until the desired dosage has been incorporated in the batch.
6. The process for making sustained period minuteincremental dosage pharmaceutical preparations which comprises intimately mixing a powdered drug and an enteric water insoluble excipient to produce a pasty mass, spreading the mass in a thin layer upon air pervious trays and drying the mass slowly without agitation in such a manner as to produce a rough granular material, breaking up .the rough granular material by light crushing, whereby to reduce it to granular particles, said mixing, drying and crushing operations constituting one cycle, and remixing the granular particles with an additional quantity of the excipient to produce a pasty mass, redrying such pasty mass slowly and without agitation in such a manner as to produce a granular material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process consisting of not less than three nor more than fifteen mixing, crushing and drying cycles repeated in successive order whereby to produce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubility in the gastro-intestinal tract, lightly crushing said finished granules to form a granular powder, forming a plurality of inert seed-like cores, placing said cores in a coating pan, rotating the coating pan, introducing thereinto a water insoluble excipient, dusting in said consisting of not less granular powder, and continuing the addition of water insoluble excipient and granular powder until the desired dosage has been incorporated in the batch.
7. The process for making sustained period minuteincremental dosage pharmaceutical preparations which comprises intimately mixing a powdered drug and an .enteric water insoluble excipient to produce a pasty material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process than three nor more than, fifteen mixing, crushing and drying cycles repeated in successive order whereby to produce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubility in the gastro-intestinal tract, lightly crushing said finished granules to form a granular powder, forming a plurality of inert seed-like cores, placing said cores in a coating pan, rotating the coating pan, introducing thereinto a water insoluble excipient, dusting in said granular powder, and continuing the addition of water insoluble excipient and granular powder' until the desired dosage has been incorporated in the batch.
8. The process for making sustained period minuteincremental dosage pharmaceutical preparations which.
comprises intimately mixing a powdered drug and an enteric water insoluble excipient to produce a pasty mass, drying the mass slowly without agitation in a hot dry atmosphere in such a manner as to produce a rough granular material, breaking up the rough granular material by light crushing, whereby to reduce it to granular particles, said mixing, drying and crushing operations constituting one cycle, and remixing the granular particles with an additional quantity of the excipient to produce a pasty mass, redrying such pasty mass slowly and without agitation in such a manner as to produce a granular material, again breaking up the rough granular material by light crushing, whereby to reduce it again to granular particles, said second mixing, drying and crushing operations constituting a second cycle, said process consisting of not less than three nor more than fifteen mixing, crushing and drying cycles repeated in successive order, whereby to produce a pharmaceutical material consisting of granules having slow but continuous and attenuated solubility in the gastrointestinal tract, lightly crushing said finished granules to form a granular powder, forming a plurality of inert seed-like cores, placing said cores in a coating pan, rotating the coating'pan, introducing thereinto a water insoluble excipient, dusting in said granular powder, and continuing the addition of water insoluble excipient and granular powder until the desired dosage has been incorporated in the batch.
9. A pharmaceutical preparation made in accordance with the process of claim'l.
10. A pharmaceutical preparation made in accordance with the process of claim 2. 1
11. A pharmaceutical preparation made in accordance with the process of claim 3.
Clarkson: Tablet Coating (New York, 1951), p. 61.

Claims (1)

1. THE PROCESS FOR MAKING SUSTAINED PERIOD MINUTE INCREMENTAL DOSAGE PHARMACEUTICAL PREPARATIONS WHICH COMPRISES INTIMATELY MIXING A POWDERED DRUG AND AN ENTRIC WATER INSOLUBLE EXCIPIENT TO PRODUCE A PASTY MASS, DRYING THE MASS SLOWLY WITHOUT AGITATION IN SUCH A MANNER AS TO PRODUCE A ROUGH GRANULAR MATERIAL, BREAKING UP THE ROUGH GRANULAR MATERIAL BY LIGHT CRUSHING, WHEREBY TO REDUCE IT TO GRANULAR PARTICLES, SAID MIXING, DRYING AND CRUSHING OPERATIONS CONSTITUTING ONE CYCLE, AND REMIXING THE GRANULAR PARTICLES WITH AN ADDITIONAL QUANTITY OF THE EXCIPIENT TO PRODUCE A PASTY MASS, REDRYING SUCH PASTY MASS SLOWLY AND WITHOUT AGITATION IN SUCH A MANNER AS TO PRODUCE A GRANULAR MATERIAL, AGAIN BREAKING UP THE ROUGH GRANULAR MATERIAL BY LIGHT CRUSHING, WHEREBY TO REDUCE IT AGAIN TO GRANULAR PARTICLES, SAID SECOND MIXING, DRYING AND CRUSHING OPERATIONS CONSTITUTING A SECOND CYCLE, SAID PROCESS CONSISTING OF NOT LESS THAN THREE NOR MORE THAN FIFTEEN MIXING, CRUSHING AND DRYING CYCLES REPEATED IN SUCCESSIVE ORDER WHEREBY TO PRODUCE A PHARMACEUTICAL MATERIAL CONSISTING OF GRANULES HAVING SLOW BUT CONTINUOUS AND ATTENUATED SOLUBILITY IN THE GASTRO-INTESTINAL TRACT, LIGHTLY CRUSHING SAID FINISHED GRANULES TO FORM A GRANULAR POWDER, FORMING A PLURALITY OF INERT SEED-LIKE CORES, PLACING SAID CORES IN A COATING PAN, ROTATING THE COATING PAN, INTRODUCING THEREINTO A WATER INSOLUBLE EXCIPIENT, DUSTING IN SAID GRANULAR POWDER, AND CONTINUING THE ADDITON OF WATER INSOLUBLE EXCIPIENT AND GRANULAR POWDER UNTIL THE DESIRED DOSAGE HAS BEEN INCORPORATED IN THE BATCH.
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US3383283A (en)*1964-01-241968-05-14Merck & Co IncMedicinal pellets coated with overlapping porous fatty acid leaflet layers
FR2444460A1 (en)*1978-12-221980-07-18Panoz DonaldControlled release oral galenical formulation - contains active components in micro-granules prepd. under high compression
US4609542A (en)*1978-12-221986-09-02Elan Corporation, P.L.C.New pharmaceutical forms for administration of medicaments by oral route, with programmed release
US4728512A (en)*1985-05-061988-03-01American Home Products CorporationFormulations providing three distinct releases
US4794001A (en)*1986-03-041988-12-27American Home Products CorporationFormulations providing three distinct releases
US4904476A (en)*1986-03-041990-02-27American Home Products CorporationFormulations providing three distinct releases
LT4844B (en)1998-07-172001-09-25Bristol-Myers Squibb CompanyEnteric coated pharmaceutical tablet and method of manufacturing
LT4843B (en)1998-05-222001-09-25Bristol-Myers Squibb Company ENTERINE COATING PHARMACEUTICAL COMPOSITION AND ITS MANUFACTURING METHOD \ t
US20040005358A1 (en)*2002-04-232004-01-08Slugg Peter H.Modified-release vasopeptidase inhibitor formulation, combinations and method
WO2009132253A1 (en)2008-04-242009-10-29Bristol-Myers Squibb CompanyUse of epothelone d in treating tau-associated diseases including alzheimer's disease
US8303988B2 (en)2000-10-132012-11-06Shionogi Inc.Antifungal once-a-day product, use and formulation thereof
EP2535044A1 (en)2006-01-272012-12-19The Regents Of the University of CaliforniaEnterically coated cysteamine, cystamine and derivatives thereof
WO2013078335A1 (en)2011-11-222013-05-30The Regents Of The University Of CaliforniaCysteamine and/or cystamine for treating ischemic injury
WO2013191965A1 (en)2012-06-182013-12-27Principia Biopharma Inc.Reversible covalent pyrrolo- or pyrazolopyrimidines useful for the treatment cancer and autoimmune diseases
WO2014004707A1 (en)2012-06-292014-01-03Principia Biopharma Inc.Formulations comprising ibrutinib
US8709491B2 (en)2011-06-282014-04-29NEOS Terapeutics, LPComposition comprising a mixture of dextro- and levo-amphetamines complexed with ion-exchange resin particles to form drug resin particles
US8747902B2 (en)2006-03-162014-06-10Tris Pharma, Inc.Modified release formulations containing drug-ion exchange resin complexes
US8889187B2 (en)2000-02-242014-11-18Shionogi Inc.Once a day amoxicillin product comprising immediate and delayed release dosage forms
US9173851B1 (en)2013-06-172015-11-03Raptor Pharmaceuticals Inc.Delayed release cysteamine bead formulation, and methods of making and using same
WO2016105531A1 (en)2014-12-242016-06-30Philip NunnSite specific dosing of a btk inhibitor
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WO2017004485A1 (en)2015-07-022017-01-05Raptor Pharmaceuticals Inc.Ado-resistant cysteamine analogs and uses thereof
WO2018005849A1 (en)2016-06-292018-01-04Principia Biopharma Inc.Modified release formulations of 2-[3-[4-amino-3-(2-fluoro-4-phenoxy-phenyl)pyrazolo[3,4-d]pyrimidin-1-yl]piperidine-1-carbonyl]-4-methyl-4-[4-(oxetan-3-yl)piperazin-1-yl]pent-2-enenitrile
US10143665B2 (en)2015-11-172018-12-04Horizon Orphan LlcMethods for storing cysteamine formulations and related methods of treatment
WO2021150476A1 (en)2020-01-202021-07-29Genzyme CorporationTherapeutic tyrosine kinase inhibitors for relapsing multiple sclerosis (rms)
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US11590081B1 (en)2017-09-242023-02-28Tris Pharma, IncExtended release amphetamine tablets
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Cited By (75)

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US4609542A (en)*1978-12-221986-09-02Elan Corporation, P.L.C.New pharmaceutical forms for administration of medicaments by oral route, with programmed release
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US4794001A (en)*1986-03-041988-12-27American Home Products CorporationFormulations providing three distinct releases
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US8889187B2 (en)2000-02-242014-11-18Shionogi Inc.Once a day amoxicillin product comprising immediate and delayed release dosage forms
US8303988B2 (en)2000-10-132012-11-06Shionogi Inc.Antifungal once-a-day product, use and formulation thereof
US20040005358A1 (en)*2002-04-232004-01-08Slugg Peter H.Modified-release vasopeptidase inhibitor formulation, combinations and method
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US11311507B2 (en)2006-01-272022-04-26The Regents Of The University Of CaliforniaEnterically coated cysteamine, cystamine and derivatives thereof
US9795578B2 (en)2006-01-272017-10-24The Regents Of The University Of CaliforniaEnterically coated cysteamine, cystamine and derivatives thereof
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US9750708B2 (en)2006-01-272017-09-05The Regents Of The University Of CaliforniaEnterically coated cysteamine, cystamine and derivatives thereof
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US9925158B2 (en)2006-01-272018-03-27The Regents Of The University Of CaliforniaEnterically coated cysteamine, cystamine and derivatives thereof
US9925156B2 (en)2006-01-272018-03-27The Regents Of The University Of CaliforniaEnterically coated cysteamine, cystamine and derivatives thereof
US10485774B2 (en)2006-01-272019-11-26The Regents Of The University Of CaliforniaEnterically coated cysteamine, cystamine and derivatives thereof
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US8747902B2 (en)2006-03-162014-06-10Tris Pharma, Inc.Modified release formulations containing drug-ion exchange resin complexes
US10668163B2 (en)2006-03-162020-06-02Tris Pharma, Inc.Modified release formulations containing drug-ion exchange resin complexes
US9675703B2 (en)2006-03-162017-06-13Tris Pharma, IncModified release formulations containing drug - ion exchange resin complexes
US9522191B2 (en)2006-03-162016-12-20Tris Pharma, Inc.Modified release formulations containing drug—ion exchange resin complexes
US9675704B2 (en)2006-03-162017-06-13Tris Pharma, Inc.Modified release formulations containing drug-ion exchange resin complexes
US9549989B2 (en)2006-03-162017-01-24Tris Pharma, IncModified release formulations containing drug-ion exchange resin complexes
WO2009132253A1 (en)2008-04-242009-10-29Bristol-Myers Squibb CompanyUse of epothelone d in treating tau-associated diseases including alzheimer's disease
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