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DK164535B - ETOPSIDE PREPARATION FOR ORAL ADMINISTRATION - Google Patents

ETOPSIDE PREPARATION FOR ORAL ADMINISTRATION Download PDF

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DK164535B
DK164535B DK122285A DK122285A DK164535B DK 164535 B DK164535 B DK 164535B DK 122285 A DK122285 A DK 122285A DK 122285 A DK122285 A DK 122285A DK 164535 B DK164535 B DK 164535B
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weight
etoposide
composition according
acid
water
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DK122285A
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DK164535C (en
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Selima Begum
Ismat Ullah
Bernard C Nunning
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Squibb Bristol Myers Co
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/70Carbohydrates; Sugars; Derivatives thereof
    • A61K31/715Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/70Carbohydrates; Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/28Steroids, e.g. cholesterol, bile acids or glycyrrhetinic acid
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4841Filling excipients; Inactive ingredients
    • A61K9/4858Organic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00Antineoplastic agents

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  • Chemical & Material Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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Description

iin

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Den foreliggende opfindelse angår etetoposidpræparat til oral administrering, der er ejendommeligt ved <£t i krav l's kendetegnende del angivne.The present invention relates to ethetoposide composition for oral administration which is characterized by <1 in the characterizing portion of claim 1.

Etoposid er et semi-syntetisk proukt afledt af podophyllotoxin.Etoposide is a semi-synthetic product derived from podophyllotoxin.

5 Dette materiale har det kemiske navn ''-demethylepipodophyllotoxin-9-(4,6-0(R)-ethyliden-jS-D-glucopyranosd). Det omtales i litteraturen som VP-16-213, VePesidR, Ethyliden-Lignm P og EPEG. Det er blevet vurderet til anvendelse i behandlingen af caicer i The National Cancer ^ Institute's regi under nr. NSC-131‘40. Det er for nylig blevet godkendt 10 af Federal Food and Drug Administration til anvendelse i behandlingen af refraktær testi kulær cancer og er blevet foreslået til anvendelse i behandlingen af småcellet lungecancer.This material has the chemical name '' -demethylpipodophyllotoxin-9- (4.6-0 (R) -ethylidene-β-D-glucopyranoside). It is referred to in the literature as VP-16-213, VePesidR, Ethylidene-Lignm P and EPEG. It has been assessed for use in the treatment of caices under the auspices of The National Cancer ^ Institute under No. NSC-131'40. It has recently been approved by the Federal Food and Drug Administration for use in the treatment of refractory testicular cancer and has been proposed for use in the treatment of small cell lung cancer.

Ved undersøgelser udført i lational Cancer Institute's regi ti Iførtes lægemidlet som en opløsning til injektion med følgende sammensæt-15 ning: etoposid 100 mg, vandfri citronsyre 10 mg, benzyl al kohol 150 mg, renset polysorbat 80 400 mg, pclyethylenglycol 300 3,25 g og absolut alkohol op til 5,12 g. Hver ampul med ovennævnte sammensætning indeholdt 5 ml opløsning, der fortyndedes 20 til 50 gange med 0,9% natriumchlorid eller 5% dextrose til injektion før administrering ved langsom intrave-20 nøs infusion.In studies conducted under the auspices of the National Cancer Institute, the drug was administered as a solution for injection with the following composition: etoposide 100 mg, anhydrous citric acid 10 mg, benzyl alcohol 150 mg, purified polysorbate 80 400 mg, pclyethylene glycol 300 3.25 g and absolute alcohol up to 5.12 g. Each ampoule of the above composition contained 5 ml of solution diluted 20 to 50 times with 0.9% sodium chloride or 5% dextrose for injection before administration by slow intravenous infusion.

Når det ovennævnte intnvenøse præparat administreredes oralt frem for ved injektion, indtoges 5 ml ampullen enten som en teskefuld dosis eller fortyndedes først med vand, og det viste sig, at biotilgængeligheden via den orale vej var ca. 90% af biotilgængeligheden via den intra-25 venøse vej (M.D'Incalci et al., Cancer Chemoterapy and Pharmacology (1982) 7:141-145). En lignende dosis taget som kapsel, hvori 100 mg aktiv bestanddel var indeholdt i ca. 1,3 ml indkapslet opløsning, hvor vehiklet bestod af polyethylenglycol 400, glycerin, vand og citronsyre, gav kun ca. halvdelen af den intravenøse opløsnings biotilgængelighed, 30 når den indtoges oralt (M. D'Incalci et al., se ovenfor). Opfindelsen løser problemet med reduceret biotilgængelighed af kapsel dosisformen og tilvejebringer en flydende formulering med tilstrækkelig høj koncentration til indkapsling, hvilken formulering giver en biotilgængelighed ved oral indgift, som er lig med den intravenøse opløsnings biotilgængelig-35 hed.When the above-mentioned intravenous formulation was administered orally rather than by injection, the 5 ml ampoule was either taken as a teaspoonful of dose or diluted first with water, and it was found that bioavailability via the oral route was about 90% of bioavailability through the intravenous route (M.D.Incalci et al., Cancer Chemotherapy and Pharmacology (1982) 7: 141-145). A similar dose taken as a capsule containing 100 mg of active ingredient for approx. 1.3 ml of encapsulated solution, in which the vehicle consisted of polyethylene glycol 400, glycerine, water and citric acid, gave only approx. half of the bioavailability of the intravenous solution when taken orally (M. D'Incalci et al., supra). The invention solves the problem of reduced bioavailability of the capsule dosage form and provides a liquid formulation of sufficiently high concentration for encapsulation which provides a bioavailability by oral administration equal to the bioavailability of the intravenous solution.

Opfindelsen drager fordel af den opdagelse, at når taurocholsyre inkluderes i et opløsningsdosispræparat med etoposid, er resultatet en markant forbedret absorption af lægemidlet efter indtagelse af præpara- 2The invention benefits from the discovery that when taurocholic acid is included in a solution dose composition with etoposide, the result is a markedly improved absorption of the drug after ingestion of the preparation.

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tet. Det antages, at dette fyldes dannelsen af en micellær opløsning af etoposid ved fortynding deri med det gastriske indhold.ment. This is believed to fill the formation of a micellar solution of etoposide by dilution therein with the gastric content.

Ved undersøgelsen af de te problem har det vist sig, at den ovenfor omtalte kapsel formulering resulterer i umiddelbar dannelse af et tungt 5 mælkehvidt bundfald, når den bandes med vand i forholdet ca. 10 ml vand pr. 100 mg etoposid. Når så lict som en lige så stor vægtmængde tauro-cholsyre i forhold til etoposidinkluderes i den flydende kapsel formulering, forsinkes bundfaldsdannelsin i mere end en time ved blanding af formuleringen med 10 ml vand. Følgende tabel illustrerer denne virkning 10 af taurocholsyre og andre galdesyier.In investigating the tea problem, it has been found that the above-mentioned capsule formulation results in immediate formation of a heavy milky white precipitate when bound with water in the ratio of approx. 10 ml water per 100 mg etoposide. When as lict as an equal amount of weight of tauro-cholic acid relative to etoposide is included in the liquid capsule formulation, the precipitate formation is delayed for more than one hour by mixing the formulation with 10 ml of water. The following table illustrates this effect 10 of taurocholic acid and other bile acids.

33

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Overfladespændingsmålinger på de vandige fortyndinger af alle gal-desyreformuleringerne omtalt i den foregående tabel har da også bekræf- . tet, at der dannes micellære opløsninger af etoposid. Dette afspejles af, at når koncentrationen af taurocholsyre i opløsningen forøges, 5 mindskes overfladespændingen indtil en vis grænse og derefter ikke yderligere. Den koncentration, hvor ingen yderligere formindskelse af overfladespændingen finder sted, omtales som den kritiske micellære koncentration.Surface tension measurements on the aqueous dilutions of all the gallic acid formulations discussed in the preceding table have also confirmed. micellar solutions of etoposide are formed. This is reflected in the fact that as the concentration of taurocholic acid in the solution is increased, the surface tension is reduced to a certain limit and then not further. The concentration at which no further reduction in surface tension occurs is referred to as the critical micellar concentration.

Fænomenet med micellær opløsning af lægemidler med ringe vandoplø-10 selighed fremkaldt af galdesyre, herunder taurocholsyre, er tidligere blevet omtalt med hensyn til griseofulvin, hexesterol, glutethimid (Bates et al., Journal of Pharmaceutical Sciences, 55, 191 - 199), re-serpin, Malone et al., ibid, 55, 972-974 (1966), fedtsyrer og cholesterol (Westergaard et al., Journal of Clinical Investigation, 58, 97-108 15 (1976))..The phenomenon of micellar dissolution of drugs with low water solubility induced by bile acid, including taurocholic acid, has been previously discussed with respect to griseofulvin, hexesterol, glutethimide (Bates et al., Journal of Pharmaceutical Sciences, 55, 191-199), re -serpin, Malone et al., ibid, 55, 972-974 (1966), fatty acids and cholesterol (Westergaard et al., Journal of Clinical Investigation, 58, 97-108 (1976)).

Den foreliggende opfindelse tilvejebringer en farmaceutisk opløsning af etoposid, der har den enestående egenskab at give en stabil "tilsyneladende opløsning" af lægemidlet ved fortynding deraf med fra 1 til 100 rumfang vand. Opløsningen er stabil og fri for bundfald i mindst 20 to timer, hvilket er tilstrækkeligt til administrering til og absorption i et pattedyrs organisme. Det har vist sig, at biotilgængeligheden af etoposid efter oral administrering af den omhandlede dosisform er i alt . væsentligt ækvivalent med den, som opnås ved intravenøs administrering af en opløsning af lægemidlet. Det antages, at indtagelsen af den om-25 handlede dosisform og den resulterende fortynding deraf med maveindhold-et resulterer i dannelsen af en micellær opløsning af etoposid i maven, der let absorberes i den gastrointestinale kanal. Ansøgerne ønsker imidlertid ikke at være bundet til nogen teoretisk forklaring på mekanismen, hvorved den enestående orale biotilgængelighed af den omhandlede formu-30 lering opnås.The present invention provides a pharmaceutical solution of etoposide having the unique property of providing a stable "apparent solution" of the drug by dilution thereof with from 1 to 100 volumes of water. The solution is stable and free from precipitation for at least 20 two hours, which is sufficient for administration to and absorption in a mammalian organism. It has been found that the bioavailability of etoposide after oral administration of the subject dosage form is total. substantially equivalent to that obtained by intravenous administration of a solution of the drug. It is believed that the ingestion of the subject dosage form and the resulting dilution thereof with the gastric contents results in the formation of a micellar solution of etoposide in the stomach which is readily absorbed in the gastrointestinal tract. However, the applicants do not wish to be bound by any theoretical explanation of the mechanism by which the unique oral bioavailability of the present formulation is achieved.

Polyethylenglykol med en molekylvægt på 200 til 400 er blevet valgt som vehikel for præparatet. Polyethylenglykol har den nødvendige opløsningskapacitet for etoposid og udviser acceptabel viskositet og disper-gerbarhed i vand til at opfylde kravene for opfindelsen. Polyethylengly-35 kol med molekylvægt på 200 til 300 foretrækkes, da det er mindre viskøst end polyethylenglykol 400. Den lavere viskositet letter fremstillingen og øger dispergerbarheden af præparatet ved blanding med vand eller ma-veindhold. Andre bestanddele i præparatet tjener til at forbedre disper- 5Polyethylene glycol having a molecular weight of 200 to 400 has been selected as the vehicle for the composition. Polyethylene glycol has the necessary dissolution capacity for etoposide and exhibits acceptable viscosity and dispersibility in water to meet the requirements of the invention. Polyethylene glycol carbon having a molecular weight of 200 to 300 is preferred since it is less viscous than polyethylene glycol 400. The lower viscosity facilitates the preparation and increases the dispersibility of the composition by admixture with water or mauve content. Other ingredients in the composition serve to improve dispersion

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gerbarheden og lette micelledannelsen ved blanding deraf med vand eller til at forbedre foreneligheden af opløsningen med kapsel skallen, når ma- . terialet indkapsles i en blød gelatinekapsel ifølge den foretrukne udførelsesform af opfindelsen.the agility and facilitate the micelle formation by mixing it with water or to improve the compatibility of the solution with the capsule shell when the terial is encapsulated in a soft gelatin capsule according to the preferred embodiment of the invention.

5 Der anvendes fortrinsvis fra 5 til 9 vægtdele polyethylenglykol 300 pr. vægtdel etoposid. Inden for dette område er etoposids opløsningshastighed tilstrækkelig til bekvem fremstilling, der opnås en tilstrækkeligt flydende blanding til bekvem håndtering, og opløsningen er tilstrækkeligt koncentreret til, at en enhedsdosisform kan indeholdes i et 10 tilstrækkeligt lille opløsningsvolumen til, at indkapsling i en blød gelatinekapsel muliggøres. Mere fortyndede opløsninger kan selvfølgelig fremstilles til dosering ved hjælp af pipette eller teske. Sådanne omfattes også af opfindelsen.Preferably from 5 to 9 parts by weight of polyethylene glycol 300 are used. part by weight of etoposide. Within this range, the dissolution rate of etoposide is sufficient for convenient preparation, a sufficient liquid mixture is obtained for convenient handling, and the solution is sufficiently concentrated to contain a unit dosage form in a sufficiently small solution volume to allow encapsulation in a soft gelatin capsule. Of course, more dilute solutions can be prepared for dosing by pipette or teaspoon. Such are also encompassed by the invention.

Etoposidet pulveriseres fortrinsvis fint før formulering til det 15 omhandlede præparat, men dette er fortrinsvis af bekvemmelighedsårsager og er ikke nødvendigt, da der dannes en sand opløsning af etoposid i polyethylenglykol . Når etoposid opløses i et vandopløseligt organisk opløsningsmiddel, og den resulterende opløsning blandes med vand, udfælder etoposidet almindeligvis på grund af dets meget lave vandopløselighed.The etoposide is preferably finely pulverized prior to formulation for the present composition, but this is preferably for convenience and is not necessary as a true solution of etoposide is formed in polyethylene glycol. When etoposide is dissolved in a water-soluble organic solvent and the resulting solution is mixed with water, the etoposide usually precipitates due to its very low water solubility.

20 Som anført indeholder præparatet taurocholsyre, og tilstedeværelsen af denne bestanddel resulterer antageligt i dannelsen af en micellær opløsning, når præparatet blandes med vand.As stated, the composition contains taurocholic acid, and the presence of this component presumably results in the formation of a micellar solution when the composition is mixed with water.

Andre galdesyrer vil ligeledes fremme dannelsen af tilsyneladende mi cell ære opløsninger ved blanding af polyethylenglykolopløsningen med 25 vand, men de er ikke egnede til anvendelse i de omhandlede præparater, da de således fremkomne micellære opløsninger er ustabile eller ikke dannes ved sure pH-værdier. Natriumdeoxycholat eller natriumcholat danner micellære opløsninger med etoposid, men de micellære opløsninger har pH-værdier på henholdsvis 10,9 og 11,0. Ved surgøring fælder etoposidet 30 ud fra sådanne opløsninger. Disse er derfor ikke egnede til oral indgift på grund af maveindholdets sure natur. Ydermere foretrækkes sure betingelser ved indkapsling i bløde gelatinekapsel skal ler, da gelatinekapslen ødelægges af ifyldte opløsninger med pH-værdier over 8,0. Ved empiriske forsøg har det vist sig, at ca. 3,5 vægtdele taurocholsyre pr. vægtdel 35 etoposid fortrinsvis er ønskværdige for tilvejebringelse af en stabil mi cel!ær opløsning ved fortynding af præparatet med vand. Mindre mængder, såsom 2,0 vægtdele, og større mængder taurocholsyre kan anvendes.Other bile acids will also promote the formation of apparent cellular solutions by mixing the polyethylene glycol solution with 25 water, but they are not suitable for use in the present compositions, since the resulting micellar solutions are unstable or not formed at acidic pH values. Sodium deoxycholate or sodium cholate forms micellar solutions with etoposide, but the micellar solutions have pH values of 10.9 and 11.0, respectively. Upon acidification, the etoposide 30 precipitates from such solutions. Therefore, these are not suitable for oral administration due to the acidic nature of the stomach contents. Furthermore, acidic conditions are preferred when encapsulated in soft gelatin capsule clay, as the gelatin capsule is destroyed by pre-filled solutions with pH values above 8.0. In empirical experiments it has been found that approx. 3.5 parts by weight of taurocholic acid per by weight of etoposide is preferably desirable to provide a stable cellular solution by diluting the composition with water. Smaller amounts such as 2.0 parts by weight and larger amounts of taurocholic acid may be used.

Det tjener intet nyttigt formål at anvende mere end ca. 10 vægtdele tau- 6It serves no useful purpose to use more than approx. 10 parts by weight of tau- 6

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rocholsyre pr. vægtdel etoposid.rocholic acid per part by weight of etoposide.

En vandopløselig syre inkluderes i præparatet for at sikre, at der . opnås en sur pH-værdi ved fortynding til dannelse af den micel lære opløsning. Af hensyn til farmaceutisk formfuldendthed og let håndtering 5 ved fremstillingen foretrækkes det at anvende en fast vandopløselig organisk carboxylsyre, men andre syrer kan anvendes. Malein-, vin-, citron-, glucon- eller ascorbinsyre, der er vandopløselige, ikke-toksiske og bekvemme at håndtere ved fremstilling af farmaceutica, foretrækkes.A water-soluble acid is included in the composition to ensure that. an acidic pH is obtained by dilution to form the micel leather solution. For pharmaceutical completeness and ease of handling in the preparation, it is preferred to use a solid water-soluble organic carboxylic acid, but other acids may be used. Maleic, tartaric, citric, gluconic or ascorbic acids which are water-soluble, non-toxic and convenient to handle in the preparation of pharmaceuticals are preferred.

Mest foretrukket er citronsyre, der har vist sig at være passende, når 10 den anvendes i mængder fra 0,1 til 0,5 vægtdele pr. vægtdel etoposid.Most preferred is citric acid which has been found to be suitable when used in amounts of 0.1 to 0.5 parts by weight per liter. part by weight of etoposide.

Det mest foretrukne forhold er 0,2 vægtdele citronsyre pr. vægtdel etoposid.The most preferred ratio is 0.2 parts by weight of citric acid per liter. part by weight of etoposide.

Ethanol tjener i præparatet det vigtige formål at tilvejebringe en hurtig dispersion ved blanding med vand og letter dannelsen af den mi-15 cellære opløsning. Andre vandopløselige, polære organiske opløsningsmidler, såsom methanol, propanol, acetone etc., der også er effektive, er ikke egnede til oral indgift, og i overensstemmelse hermed er ethanol blevet valgt til dette formål. Mindst 5 vægtprocent ethanol i præparatet er nødvendigt til dette formål, men højere mængder, op til 20 vægtpro-20 cent, kan anvendes, især i tilfælde af pipette- eller teskefulddoseringsformer. Til indkapsling i en blød gelatinekapsel kan der maksimalt anvendes 10 vægtprocent ethanol i præparatet. Opløsninger med højere koncentrationer af ethanol end 10 vægtprocent kan fremkalde dehydrering af gelatinekapsel væggen og er følgelig ikke egnede til indkapsling i 25 denne type kapsel.Ethanol in the composition serves the important purpose of providing a rapid dispersion by mixing with water and facilitates the formation of the micellar solution. Other water-soluble polar organic solvents such as methanol, propanol, acetone etc. which are also effective are not suitable for oral administration and accordingly ethanol has been selected for this purpose. At least 5% by weight of ethanol in the composition is necessary for this purpose, but higher amounts, up to 20% by weight, can be used, especially in the case of pipette or teaspoon dosage forms. For encapsulation in a soft gelatin capsule, a maximum of 10 weight percent ethanol can be used in the preparation. Solutions with ethanol concentrations higher than 10% by weight can cause dehydration of the gelatin capsule wall and are therefore not suitable for encapsulation in this type of capsule.

Til anvendelse af det omhandlede præparat i enhedsdosisform indeholdt i en blød gelatinekapsel er det sluttelig ønskværdigt at inkludere op til ca. en vægtdel vand pr. vægtdel etoposid for at forbedre foreneligheden af præparatet med den bløde gelatinekapsel skal. Den hydrofi-30 le natur af polyethylenglykol, ethanol, citronsyre og taurocholsyre gør, at præparatet uddrager vandet fra kapsel skallen, og kan bevirke, at denne ødelægges ved længere opbevaring. I præparatet inkluderes der derfor vand i tilstrækkelig mængde, fortrinsvis en vægtdel vand pr. vægtdel etoposid, til at gøre præparatet foreneligt med kapselskallen og fore-35 bygge dehydrering deraf. Det er ønskværdigt at vælge en mængde vand, der vil give stabilitet i en opbevaringsperiode på 2 år ved stuetemperatur, når kapslen opbevares i en lukket beholder.Finally, for use of the present unit dosage formulation contained in a soft gelatin capsule, it is desirable to include up to approx. one part by weight of water per part by weight etoposide to improve the compatibility of the composition with the soft gelatin capsule. The hydrophilic nature of polyethylene glycol, ethanol, citric acid and taurocholic acid causes the preparation to extract the water from the capsule shell, and can cause it to be destroyed by longer storage. Therefore, the composition includes water in sufficient quantity, preferably one part by weight of water per day. part by weight of etoposide to make the composition compatible with the capsule shell and prevent dehydration thereof. It is desirable to select an amount of water that will provide stability for a storage period of 2 years at room temperature when the capsule is stored in a sealed container.

De foretrukne udførelsesformer af præparatet ifølge opfindelsen er 7The preferred embodiments of the composition of the invention are 7

DK 164535 BDK 164535 B

stabile, flydende præparater i form af sande opløsninger med følgende sammensætning.stable, liquid preparations in the form of true solutions of the following composition.

Bestanddel Vægtdele 5 polyethylenglykol 300 5 til 9 etoposid 1 citronsyre 0,1 til 0,5 taurocholsyre 2,0 til 10Ingredient Weight parts 5 polyethylene glycol 300 5 to 9 etoposide 1 citric acid 0.1 to 0.5 taurocholic acid 2.0 to 10

Ethanol 5 til 20 vægtprocent af 10 opløsningens samlede vægtEthanol 5 to 20% by weight of the total weight of the solution

Den mest foretrukne udførelsesform af præparatet ifølge opfindelsen er følgende sammensætning: 15 Bestanddel Væqtdele polyethylenglykol 300 5,8 etoposid, fint pulveriseret 1,0 citronsyre 0,2 ethanol 1,0 20 taurocholsyre 3,5 vand 1,0The most preferred embodiment of the composition of the invention is the following composition: Component Weight parts polyethylene glycol 300 5.8 etoposide, finely powdered 1.0 citric acid 0.2 ethanol 1.0 20 taurocholic acid 3.5 water 1.0

Den foretrukne sammensætning ifølge opfindelsen belyses nærmere i det følgende eksempel.The preferred composition of the invention is elucidated in the following example.

2525

Eksempel Følgende bestanddele afvejedes: 30 etoposid 25,0 g citronsyre, vandfri, USP 5,0 g polyethylenglykol 300 170,0 g ethanol, USP 25,0 g taurocholsyre 87,5 g 35 renset vand, USP 25,0 gExample The following ingredients were weighed: etoposide 25.0 g citric acid, anhydrous, USP 5.0 g polyethylene glycol 300 170.0 g ethanol, USP 25.0 g taurocholic acid 87.5 g purified water, USP 25.0 g

Taurocholsyren sættes portionsvis til polyethylenglykol 300 under omrøring til dannelse af en suspension. Vandet tilsættes dernæst, efter-The taurocholic acid is added portionwise to polyethylene glycol 300 with stirring to form a suspension. The water is then added, after-

DK 164535 BDK 164535 B

8 fulgt af ethanolen og citronsyren. Der dannes en opløsning, som opvarmes til 65°C, tillades at afkøle til 35eC, og filtreres ("Mil 1ipore AP 25 29325"). En atmosfære af nitrogen opretholdes over opløsningen under disse trin. Filtratet holdes ved 30-35eC, og etoposidet opløses dernæst 5 deri. Opløsningen analyseres dernæst (fundet: 71,3 mg etoposid pr. g) og fyldes i bløde gelatinekapsler med 100 mg etoposid pr. kapsel.8 followed by the ethanol and citric acid. A solution is formed which is heated to 65 ° C, allowed to cool to 35 ° C, and filtered ("Mil 1ipore AP 25 29325"). An atmosphere of nitrogen is maintained over the solution during these steps. The filtrate is maintained at 30-35 ° C and the etoposide is then dissolved therein. The solution is then analyzed (found: 71.3 mg etoposide per g) and filled into soft gelatin capsules with 100 mg etoposide per g. capsule.

Den ovennævnte kapselfyldningsopløsning har følgende karakteristika og stabilitet:The above capsule filling solution has the following characteristics and stability:

10 KARAKTERISTIKA10 CHARACTERISTICS

1. Farve mørkebrun 2. pH 4,6 3. Viskositet tilfredsstillende 15 4. Dispergerbarhed let dispergerbar 5. Skal forenelighed, fysisk forenelig 6. Bundfaldsdannelsestid ved fortynding med Η£θ til 1:1, >3 timer 1:5, 1:10 og 1:100.1. Color dark brown 2. pH 4.6 3. Viscosity satisfactory 4. Dispersibility easily dispersible 5. Must be compatible, physically compatible 6. Precipitation time by dilution with Η £ θ to 1: 1,> 3 hours 1: 5, 1: 10 and 1: 100.

2020

StabilitetStability

Opbevaringstemperatur Opbevaringstid % tilbageværende (dage) 25 4eC (kontrol) 8 100 70°C 5 102 70eC 8 102 56eC 8 102 30 37eC 8 105 25°C 8 99Storage temperature Storage time% remaining (days) 25 4eC (control) 8 100 70 ° C 5 102 70eC 8 102 56eC 8 102 30 37eC 8 105 25 ° C 8 99

Claims (14)

1. Etoposidpræparat til oral administrering, KENDETEGNET ved, at det indeholder etoposid, polyethylenglykol, taurocholsyre, ethanol og en 5 vandopløselig syre, idet mængden af taurocholsyre er fra 1 til ca. 10 vægtdele pr. vægtdel etoposid, og komponenterne i øvrigt forefindes i sådanne forhold, at der dannes en homogen væske.1. Ethoposide composition for oral administration, CHARACTERIZED in that it contains etoposide, polyethylene glycol, taurocholic acid, ethanol and a water-soluble acid, the amount of taurocholic acid being from 1 to about 10 parts by weight per part by weight of etoposide, and the components are otherwise present in such conditions that a homogeneous liquid is formed. 2. Præparat ifølge krav 1, KENDETEGNET ved, at det er på enheds- 10 dosisform, hvor den homogene væske er indeholdt i en blød gelatinekapsel .2. A composition according to claim 1, characterized in that it is in unit dosage form wherein the homogeneous liquid is contained in a soft gelatin capsule. 3. Præparat ifølge krav 2, KENDETEGNET ved, at enhedsdosen indeholder fra 10 mg til 100 mg etoposid. 153. A composition according to claim 2, characterized in that the unit dose contains from 10 mg to 100 mg etoposide. 15 4. Præparat ifølge krav 2, KENDETEGNET ved, at den homogene væske også indeholder vand i en mængde, som er tilstrækkelig til at forhindre dehydrering af kapsel skal len og gøre kapsel skallen stabil i en opbevaringsperiode på mindst 2 år i en lukket beholder ved stuetemperatur. 204. A composition according to claim 2, characterized in that the homogeneous liquid also contains water in an amount sufficient to prevent capsule dehydration and to make the capsule shell stable for at least 2 years in a closed container at room temperature. . 20 5. Præparat ifølge krav 1, KENDETEGNET ved, at molekylevægten af polyethylenglykolen er i området fra ca. 200 til ca. 400.5. A composition according to claim 1, characterized in that the molecular weight of the polyethylene glycol is in the range of from about. 200 to approx. 400th 6. Præparat ifølge krav 1, KENDETEGNET ved, at molekylvægten af 25 polyethylenglykolen er ca. 300.6. A composition according to claim 1, characterized in that the molecular weight of the polyethylene glycol is approx. 300th 7. Præparat ifølge krav 6, KENDETEGNET ved, at vægtmængden af polyethylenglykol en er fra 5 til 9 gange vægtmængden af etoposid.A composition according to claim 6, characterized in that the weight amount of polyethylene glycol is from 5 to 9 times the weight amount of etoposide. 8. Præparat ifølge krav 1, KENDETEGNET ved, at den vandopløselige syre er en ikke-toksisk organisk carboxylsyre.A composition according to claim 1, characterized in that the water-soluble acid is a non-toxic organic carboxylic acid. 9. Præparat ifølge krav 1, KENDETEGNET ved, at den vandopløselige syre er citronsyre. 35A composition according to claim 1, characterized in that the water-soluble acid is citric acid. 35 10 Bestanddel Vægtdele polyethylenglykol 300 5 til 9 etoposid 1 citronsyre 0,1 til 0,5 taurocholsyre 2,0 til 10 15 ethanol 5 til 20 vægtprocent af præparatet10 Component Weight parts polyethylene glycol 300 5 to 9 etoposide 1 citric acid 0.1 to 0.5 taurocholic acid 2.0 to 10 15 ethanol 5 to 20% by weight of the composition 10. Præparat ifølge krav 1, KENDETEGNET ved, at det indeholder 2,0 til 10 vægtdele taurocholsyre pr. vægtdel etoposid. DK 164535 BA composition according to claim 1, characterized in that it contains 2.0 to 10 parts by weight of taurocholic acid per day. part by weight of etoposide. DK 164535 B 11. Præparat ifølge krav 1, KENDETEGNET ved, at det indeholder 3,5 vægtdele taurocholsyre pr. vægtdel etoposid.11. A composition according to claim 1, characterized in that it contains 3.5 parts by weight of taurocholic acid per day. part by weight of etoposide. 12. Præparat ifølge krav 1, KENDETEGNET ved, at mængden af ethanol 5 er fra 5 til 20 vægtprocent.A composition according to claim 1, characterized in that the amount of ethanol 5 is from 5 to 20% by weight. 13. Præparat ifølge krav 1, KENDETEGNET ved, at det omfatter en opløsning med følgende sammensætning:A composition according to claim 1, characterized in that it comprises a solution of the following composition: 14. Præparat ifølge krav 13, KENDETEGNET ved, at det omfatter en opløsning tilpasset indkapsling i en blød gelatineskal og med følgende 20 sammensætning: Bestanddel Vægtdele polyethylenglykol 300 6,8 etoposid, fint pulveriseret 1,0 25 citronsyre 0,2 ethanol 1,0 taurocholsyre 3,5 vand 1,0 30 35A composition according to claim 13, characterized in that it comprises a solution adapted to encapsulation in a soft gelatin shell and having the following composition: Component Weight parts polyethylene glycol 300 6.8 etoposide, finely powdered 1.0 citric acid 0.2 ethanol 1.0 taurocholic acid 3.5 water 1.0 30 35
DK122285A 1984-03-19 1985-03-18 ETOPSIDE PREPARATION FOR ORAL ADMINISTRATION DK164535C (en)

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JPS61189230A (en) * 1985-02-19 1986-08-22 Nippon Kayaku Co Ltd Etoposide preparation
DE3629386A1 (en) * 1986-08-29 1988-03-03 Scherer Gmbh R P GELATINE CAPSULES AND METHOD FOR THEIR PRODUCTION
US4927638A (en) * 1986-10-08 1990-05-22 Bristol-Myers Company Etoposide solutions
US5154930A (en) * 1987-03-05 1992-10-13 The Liposome Company, Inc. Pharmacological agent-lipid solution preparation
US5376381A (en) * 1988-02-25 1994-12-27 The Liposome Company, Inc. Integrity protected gelatin
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FR2358144A1 (en) * 1976-07-13 1978-02-10 Lipha Compsn. for treating biliary lithiasis - contains hymecromone and chenodeoxy-cholic acid, with lower cost and better tolerance
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