Development and validation of a RP-HPLC method for determination of atorvastatin calcium and aspirin in a capsule dosage form
ABSTRACT A simple, specific and accurate reverse phase high performance liquid chromatographic method was developed for the simultaneous determination of atorvastatin calcium and aspirin in capsule dosage forms. A phenomenex Gemini C-18, 5 mm column having 250 x 4.6 mm i.d. in isocratic mode, with mobile phase containing 0.02 M potassiumdihydrogen phosphate: methanol (20:80) adjusted to pH 4 using ortho phosphoric acid was used. The flow rate was 1.0 ml/ min and effluents were monitored at 240 nm. The retention times of atorvastatin calcium and aspirin were 5.4 min and 3.4 min, respectively. The linearity for atorvastatin calcium and aspirin were in the range of 0.5-4 mg/ml and 5-25 mg/ml, respectively. The recoveries of atorvastatin calcium and aspirin were found to be in the range of 98.02-100.68% and 98.38-101.42%, respectively. The proposed method was validated and successfully applied to the estimation of atorvastatin calcium and aspirin in combined capsule dosage forms.
SourceAvailable from: Safwan Ashour
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ABSTRACT: A new rapid and sensitive high performance liquid chromatography (HPLC) method has been developed for the simultaneous determination of atorvastatin—an antihyperlipidemic drug along with most commonly prescribed drugs (antihyperlipidemic, antihypertensive, antidiabetic, antithrombotic) in bulk and marketed combined formulations. The chromatographic separation was carried out by gradient elution mode with acetonitrile as organic modifier and 0.1% triethylamine acetate (TEAA) buffer pH 5 at a flow rate of 1 mL/min and a diode array detector at wavelength 230 nm was employed for detection of the analytes. Calibration curves were linear in the range of 5–150 μg/mL for all the drugs with correlation coefficients of determination (r2 values)≥0.999. Limits of detection (LODs) and Limits of quantification (LOQs) ranged from 0.1 to 0.27 μg/mL and 0.3 to 0.89 μg/mL respectively. Intra-day and inter-day precision was studied at three concentration levels (20, 60 and 100 μg/mL). The intra-day and inter-day RSD for all compounds was less than 2.0%. The accuracy for all compounds was found to be between 98% and 102%. Thus, the performance of the method described allows its use in quantification of atorvastatin along with 9 most commonly prescribed drugs available in market as atorvastatin combined dosage forms.08/2012; 2(4):285–292. DOI:10.1016/j.jpha.2012.02.006
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ABSTRACT: Simple, accurate, precise, sensitive, and validated high-performance liquid chromatography (HPLC) and high-performance thin-layer chromatography (HPTLC)-densitometric methods were developed for simultaneous determination of fenofibrate (FEN), atorvastatin (ATO), and ezetimibe (EZE) in combined tablet dosage form. In Method A, the gradient RP-HPLC analysis was performed on a Shim-pack C18 column (150 x 6 mm id), using a mobile phase consisting of 0.1% formic acid and acetonitrile in solvent gradient elution for 25 min at a flow rate of 1.5 mL min(-1). Quantification was carried out using a photodiode array UV detector at 245 nm. The employment of diode array detector allowed selectivity confirmation by peak purity evaluation. In Method B, the HPTLC analysis was carried out on an aluminum-backed sheet of silica gel 60F(254) layer using toluene: methanol: triethylamine (8:1.5:0.1, v/v/v) as the mobile phase. Quantification was achieved with UV densitometry at 245 nm. The analytical methods were validated according to International Conference on Harmonization guidelines. Low relative standard deviation values indicated good precision. Both the methods were successfully applied for the analysis of drugs in laboratory-prepared mixtures and commercial tablets. No chromatographic interference from tablet excipients was found, and hence these methods are applicable for simultaneous determination of FEN, ATO, and EZE in pharmaceutical formulations.Journal of Liquid Chromatography & Related Technologies 06/2014; 37(19). DOI:10.1080/10826076.2013.873870 · 0.64 Impact Factor