LC determination of rosiglitazone in bulk and pharmaceutical formulation.
ABSTRACT An isocratic reversed phase liquid chromatographic (RP-LC) method has been developed and subsequently validated for the determination of rosiglitazone and its related impurities. Separation was achieved with a Symmetry C18 column and sodium phosphate buffer (pH adjusted to 6.2):acetonitrile (50:50, v/v) as eluent, at a flow rate of 1.0 ml/min. UV detection was performed at 245 nm. The method is simple, rapid, selective and stability indicating. Indole was used as internal standard for the purpose of quantification of rosiglitazone. The described method is linear over a range of 0.45-10 microg/ml for related impurities and 180-910 microg/ml for assay of rosiglitazone. The method precision for the determination of assay and related compounds was below 1.0 and 3.6% RSD, respectively. The mean recoveries of impurities were found to be in the range of 95-102%. The percentage recoveries of Active Pharmaceutical Ingredient (API) from dosage forms ranged from 99.02 to 101.30. The method is useful in the quality control of bulk manufacturing and also in pharmaceutical formulations.
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ABSTRACT: A simple, rapid, and precise reversed-phase liquid chromatographic method is developed for the simultaneous determination of metformin in combination with rosiglitazone. This method uses a Zorbax XDB C(18) 15-cm analytical column, a mobile phase of acetonitrile and buffer containing 10mM disodium hydrogen phsosphate, and 5mM sodium dodecyl sulphate in the ratio of 34:66 (v/v), and pH is adjusted to 7.1 with orthophosphoric acid. The instrumental settings are a flow rate of 1 mL/min, column temperature at 40 degrees C, and detector wavelength of 226 nm. The internal standard method is used for the quantitation of metformin and rosiglitazone. Methylparaben is used as an internal standard. The method is validated and shown to be linear. The correlation coefficients for metformin and rosiglitazone are 0.9996 and 0.9997, respectively. The relative standard deviation for six replicate measurements in two sets of each drug in the tablets is always less than 2%.Journal of chromatographic science 03/2004; 42(2):70-3. · 0.79 Impact Factor
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ABSTRACT: The objective of the study was to improve the oral therapeutic efficacy a formulation has been designed which contains two drug i.e glimepiride and metformin Hcl as well as to make a common analytical method for quantitative combined drug estimation. An object of the present invention is to provide a dosage form comprising of an active ingredient as modified release and an active ingredient as immediate release, wherein the modified release active ingredient is selected from high dose API and the immediate release active ingredient is selected from low dose active ingredients. Using HPMCk-100m ,povidone k 90 D and MCC modified dosage form has been formulated by wet granulation method . Tablet compressing was done with core rod tooling in which only one surface of core is expose to outside and other drug is incorporated in cup portion. Calibration curve for glimepiride, metformin hcl was plotted by taking phosphate methanol:D.water :1:98 as a blank which shows an absorption maxima at 228nm & 237nm.Simuntaneous estimation of two drug during invitro dissolution also carried out. The % drug release for glimepiride as immediate release is 98.1.Metformin Hcl releases in 4 hours ,8 hours and 12 hours 61.5%,90.3% and 99.6% respectively.Journal of Pharmacy Research. 01/2010;
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ABSTRACT: A simple, selective and robust reverse phase high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (ESI-MS/MS) method for simultaneous quantitation of pioglitazone (PIO), pioglitazone metabolite M-IV - hydroxypioglitazone (OH-PIO) and metformin (MET) in human plasma using deuterated internal standards (IS) is developed and fully validated as per industrial practices. After acetonitrile-induced protein precipitation of the plasma samples; PIO, OH-PIO, MET and IS were chromatographed on reverse phase column and analyzed in the multiple reaction monitoring in positive ion mode. The ion transitions were monitored at m/z 357.2→134.2 for PIO, 373.0→150.1 for OH-PIO, 130.2→71.0 for MET, 361.1→134.2 for PIO-IS and 136.1→77.1 for MET-IS. The total chromatographic run time was 4.0min. A linear response function (r>0.998) was established for the range of concentrations 15-2500ng/mL, 10-1500ng/mL and 25-3000ng/mL for PIO, OH-PIO and MET respectively in human plasma. The intra and inter-day precision and accuracy values have met the set acceptance criteria. The method is simple, selective, robust economic and has been applied successfully to more than 2000 plasma samples as part of pharmacokinetic study in humans.Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 05/2013; 930C:136-145. · 2.78 Impact Factor