Current Issue : July - September Volume : 2017 Issue Number : 3 Articles : 5 Articles
A simple, isocratic and robust RP-HPLC method for the analysis of azithromycin was\ndeveloped, validated and applied for the analysis of bulk samples, tablets and suspensions.\nThe optimum chromatographic conditions for separation were established as a mobile phase\ncomprised of acetonitrile-0.1 M KH2PO4 pH 6.5ââ?¬â??0.1 M tetrabutyl ammonium hydroxide pH 6.5-water\n(25:15:1:59 v/v/v/v) delivered at a flow rate of 1.0 mL/min. The stationary phase consisted of\nreverse-phase XTerraÃ?® (250 mm Ã?â?? 4.6 mm i.d., 5 Ã?¼m particle size) maintained at a temperature of\n43 ââ??¦C with a UV detection at 215 nm. The method was found to be linear in the range 50%ââ?¬â??150%\n(r2 = 0.997). The limits of detection and quantification were found to be 0.02% (20 Ã?¼g) and 0.078%\n(78 Ã?¼g), respectively, with a 100.7% recovery of azithromycin. Degradation products of azithromycin\nin acidic and oxidative environments at 37 ââ??¦C were resolved from the active pharmaceutical ingredient\nand thus the method is fit for the purpose of drug stability confirmation....
A simple, precise, accurate and economical UV visible spectrophotometric method has been developed for estimation of ofloxacin drug by AUC method. The standard and sample solutions were prepared by using double distilled water as a solvent. Quantitative determination of the drug was performed at wavelength range 276-300 nm. The linearity was established over the concentration range of 02-10 µg/ml for ofloxacin with correlation coefficient value of 0.993 Precision studies showed that % relative standard deviation was within range of acceptable limits. The mean percentage recovery was found to be 100%. The proposed method has been validated as per ICH guidelines....
The aim of this study is the identification, structural characterization, and qualification of a degradation impurity of bisoprolol\nlabeled as Impurity RRT 0.95. This degradation product is considered as a principal thermal degradation impurity identified in\nbisoprolol film-coated tablets. The impurity has been observed in the stress thermal degradation study of the drug product. Using\nHPLC/DAD/ESI-MS method, a tentative structure was assigned and afterwards confirmed by detailed structural characterization\nusing NMR spectroscopy.The structure of the target Impurity RRT 0.95 was elucidated as phosphomonoester of bisoprolol, having\nrelative molecular mass of 406 (positive ionizationmode).Thestructural characterization was followed by qualification of Impurity\nRRT 0.95 using several different in silico methodologies. Fromthe results obtained, it can be concluded that no new structural alerts\nhave been generated for Impurity RRT 0.95 relative to the parent compound bisoprolol. The current study presents an in-depth\nanalysis of the full characterization and qualification of an unidentified impurity in a drug product with the purpose of properly\ndefining the quality specification of the product....
Imatinib mesylate exhibits many polymorphic forms and most stable and commercialized polymorphs are α and β forms. Molecules in α and β polymorphic forms exhibit significant conformational differences due to their different intra- and intermolecular interactions, which stabilize their molecular conformations and affect their physicochemical properties such as bulk density, melting point, solubility, stability and process-ability. The manufacturing process of a drug tablet included granulation, compression, coating and drying may cause polymorphic conversions. Therefore, polymorphic content of the drug substance should be controlled during quality control and stability testing. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, Differential Scanning Calorimetry (DSC) and powder X-ray diffraction (PXRD) methods were evaluated for determination of the polymorphic content of the drug substance and drug product. PXRD was the most accurate technique over the other two and selected as a preferred method and is used as validation method. In the present study, quantification PXRD and DSC methods have been developed to determine the amount of β-polymorphic form in α polymorph of imatinib mesylate tablets 400 mg and 100 mg. Mixtures with different ratios of α and β forms were scanned using X-ray diffractometer with a time per step(s) 1000 over an angular range of 19.9–21.0° 2θ and the peak heights for characteristic peak of β form at 20.5±0.2° 2θ diffraction angle were used to generate a calibration curve. The detection limit of β polymorph in α form imatinib mesylate tablets was found as 0.5% and the linear regression analysis data for the calibration plots showed good linear relationship with correlation coefficient of 0.9999 with respect to relative peak height in the concentration range of 1–30 wt% β form containing tablet mixtures. The obtained results at each stage of the validation study proved that the method is specific, repeatable, precise and accurate and could be used for determination of β polymorph content in tablets produced by using α polymorph of imatinib mesylate. The developed PXRD quantification method was used to monitor the polymorphic purity of α form drug substance and corresponding drug products during the quality control analyses and stability studies....
This work represents development and validation of novel, accurate, precise, rugged, robust and reproducible high performance thin-layer chromatographic technique for the simultaneous estimation of metoprolol succinate and chlorthalidone from marketed formulation. High performance thin-layer chromatography was performed using HPTLC aluminium plates precoated silica gel plate 60 F254 as stationary phase. The solvent system consisted of Toluene: Ethyl acetate: Methanol: Triethylamine (6: 1: 1: 0.6 v/v/v/v) as the mobile phase for the separation of metoprolol succinate and chlorthalidone. The densitometric analysis of metoprolol succinate and chlorthalidone was carried out at 230 nm. The method was validated as per the International Conference on Harmonization (ICH) guidelines and found to be linear in the range of 500-7000 ng spot−1 for metoprolol succinate and 125-1750 ng spot−1 for chlorthalidone. Rf value for metoprolol succinate and chlorthalidone is 0.53 and 0.24 respectively. The relative standard deviation (% RSD) values of the precision study were <2% which indicated that the developed method was precise; recovery was found to be 99.9% - 100.1% for metoprolol succinate and 99.9% - 100.3% chlorthalidone respectively. The extremely simple mobile phase composition makes this method cost effective, rapid and nontedious. The method can be important tool for simultaneous estimation of both drugs in commercial products for routine analysis and quality control laboratories....
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