The validation of a microbiological assay applying the cylinder-plate method to determine the quinolone gemifloxacin mesylate (GFM) content is described. Using a strain of Staphylococcus epidermidis ATCC 12228 as the test organism, the GFM content in tablets at concentrations ranging from 0.5 to 4.5 μg mL(-1) could be determined. A standard curve was obtained by plotting three values derived from the diameters of the growth inhibition zone. A prospective validation showed that the method developed is linear (r=0.9966), precise (repeatability and intermediate precision), accurate (100.63%), specific and robust. GFM solutions (from the drug product) exposed to direct UVA radiation (352 nm), alkaline hydrolysis, acid hydrolysis, thermal stress, hydrogen peroxide causing oxidation, and a synthetic impurity were used to evaluate the specificity of the bioassay. The bioassay and the previously validated high performance liquid chromatographic (HPLC) method were compared using Student's t test, which indicated that there was no statistically significant difference between these two validated methods. These studies demonstrate the validity of the proposed bioassay, which allows reliable quantification of GFM in tablets and can be used as a useful alternative methodology for GFM analysis in stability studies and routine quality control. The GFM reference standard (RS), photodegraded GFM RS, and synthetic impurity samples were also studied in order to determine the preliminary in vitro cytotoxicity to peripheral blood mononuclear cells. The results indicated that the GFM RS and photodegraded GFM RS were potentially more cytotoxic than the synthetic impurity under the conditions of analysis applied.

Recebido em 20/6/08; aceito em 14/1/09; publicado na web em 28/5/09 A dissolution test for telithromycin tablets was validated and developed. In order to choose the most discriminatory one, the conditions to carry out are 900 mL of sodium phosphate buffer at pH 7.5, paddles at 50 rpm stirring speed, time test set to 60 min and using USP apparatus 2 with paddles. The UV spectrophotometric method for determination of telithromycin released was developed and validated. The method presents linearity (r = 1) in the concentration range of 20-60 μg/mL. Precision and recoveries were good, 100.62 and 97.06%, respectively. The method was successfully used for the dissolution test of telithromycin tablets.

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Nitazoxanide is a new broad-spectrum, antiparasitic drug agent. The photodegradation of nitazoxanide was studied in order to investigate the degradation kinetics of this drug. The analyses of the degraded samples were performed by a stability-indicating liquid chromatographic method. The degradation was carried out in acetonitrile with coated tablets or oral suspension powder in quartz cells under UVC light at 254 nm. The kinetics parameters, such as order of reaction, rate constants, half-life (t(1/2)), and the time when 90% of the drug original concentration was left, were determined. The photodegradation of nitazoxanide for both pharmaceutical formulations in acetonitrile solution shows a zero-order kinetics under the applied experimental conditions. The obtained results confirm the reliability of the chromatographic method for determining the kinetics run of nitazoxanide in the presence of its degradation products. The present study reveals the photolability of the drug in solution. Thus, appropriated photoprotection is recommended during the manipulation of the drug.