Process for the preparation of oral compositions containing quin

Drug – bio-affecting and body treating compositions – Preparations characterized by special physical form – Tablets – lozenges – or pills

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424470, 424474, 264115, 264117, 264118, 264122, 514311, 514781, 514960, A61K 3144, A61K 3147, A61K 31495, A61K 920

Patent

active

058403337

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BRIEF SUMMARY
The present invention relates to a process for the preparation of an oral formulation of products belonging to the quinolone family.
The products of the quinolone family are widely known antibacterial agents, which have been described in particular in the following references: BE 870 576; U.S. Pat. No. 4,448,962; DE 3 142 854; EP 047 005; EP 206 283; BE 887 574; EP 221 463; EP 140 116; EP 131 839; EP 154 780; EP 078 362; EP 310 849; EP 520 240; U.S. Pat. No. 4,499,091; U.S. Pat. No. 4,704,459; U.S. Pat. No. 4,795,751; U.S. Pat. No. 4,668,784.
The preparation of fine granules by a wet granulation process has been described in the publication by Y. Shirai et al., Biol. Pharm. Bull. 16(2), 172 (1993).
A process for the direct compression of the mixture of a quinolone with excipients, without the prior addition of mixing water, has been described in Patent EP 189,114.
However, the previously known processes have drawbacks which lead, most often, to an imperfect result. Indeed, the processes which make use of wet granulation have a tendency to slow down the dissolution and to promote the formation of hydrates, which are less soluble or more difficult to disperse when compared with the corresponding anhydrous form. This results in a delay in the dissolution and the release of the active principle, which may be a nuisance in the use of antimicrobial medicinal products. Moreover, methods for the direct compression of a mixture of the excipients in powder form has the advantage of avoiding the formation of hydrates, but the quality of the tablets obtained is not always consistent and satisfactory insofar as cleavage problems arise, thus rendering some batches of tablets unsuitable for marketing. Industrial losses, which may prove to be considerable, are thereby incurred.
It has now been found that oral formulations of active principles belonging to the quinolone family, having no problems of overly slow solubilization or any cleavage problems, could be prepared by incorporating an intermediate step of compacting and then of grinding. Namely, by dry-mixing the said active principle with the suitable excipients for an oral formulation, followed by a compacting, a grinding and then compression of the granules thus obtained. The new step of compacting and grinding makes it possible to carry out the direct compression of a powder of much coarser particle size and leads to tablets having no cleavage problems. The industrial risks due to batch-to-batch variations were thus able to be reduced, or even eliminated.
According to the invention, the products of quinolone family may be chosen from the products of general formula: ##STR1## in which R.sub.1 is an alkyl radical containing 1 to 4 carbon atoms or a fluoroethyl, cyclopropyl, methylamino or difluorophenyl radical, X represents a nitrogen atom or a group .dbd.CR.sub.7 -- in which R.sub.7 is a hydrogen, chlorine or fluorine atom or alternatively R.sub.7 forms, with the radical R.sub.1 and the atoms to which they are attached, a 6-membered heterocycle which is substituted with a methyl radical and which optionally contains an oxygen or sulphur atom, R.sub.2 is a hydrogen atom or may represent an amino radical if R.sub.7 is a fluorine atom, and radical of structure: ##STR2## in which R.sub.4, R.sub.5 and R.sub.6 are identical or different and represent hydrogen atoms or methyl radicals, or the pharmaceutically acceptable salts thereof.
More especially advantageous among the quinolones mentioned above are pefloxacin, sparfloxacin, ciprofloxacin, ofloxacin, levofloxacin, enoxacin, norfloxacin, fleroxacin, lomefloxacin, temafloxacin, amifloxacin, tosufloxacin, flumequine, rufloxacin, clinafloxacin, Bay-y-3118 and PD 131 628.
According to the process of the invention, the compacting is carried out by subjecting the product to a mechanical densification at a rather low force, followed by grinding the agglomerates thus obtained on a grid, in order to obtain a mixture having a particle size of 50 .mu.m to 1 mm and preferably greater than 100 .mu.m, thus allowing a good flow and g

REFERENCES:
patent: 4639458 (1987-01-01), Katdare
patent: 4973470 (1990-11-01), Mills et al.
English language Derwent Abstract of JP 1175936.

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