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An isocratic reversed-phase high-performance liquid chromatographic method has been developed and validated for the simultaneous determination of aspirin, prasugrel HCl and clopidogrel bisulfate in the presence of clopidogrel-related compound (impurity-A) in focus on counterfeit. This method was used to determine counterfeited antiplatelet drugs in two substandard Indian pharmaceutical products sold on the market in Yemen and two traditional herbal medicines sold on the market in China. Thin layer chromatography and mass spectrometry of counterfeit herbal medicines have additionally been carried out to verify the identification of adulterants. Chromatographic separation was performed on Inertsil ® ODS-3 C18 (4.6 × 250 mm, 5 μm) with isocratic mobile phase elution containing a mixture of acetonitrile: (25 mM) potassium dihydrogen phosphate buffer, pH 2.7 adjusted with 0.1 M o -phosphoric acid (79: 21, v/v), at a flow rate of 1 mL/min and UV detection at 220 nm. Designs of experiment methodology, Plackett–Burman and Box–Behnken designs were used for the screening and optimization of the mobile phase composition. The method validation was also performed in accordance with the International Council on Harmonization (ICH) guidelines. The method developed for routine analysis was found to be sensitive, simple, accurate and highly robust. The results were statistically compared to reference methods using Student's t -test and variance ratio F -test at P  < 0.05. [ABSTRACT FROM AUTHOR]

Aspirin (ASP) (analgesic; anti-inflammatory; anti-platelet), clopidogrel bisulphate (CLP) (anti-platelet) and atorvastatin calcium (ATV) (anti-hyperlipidemia) are co-formulated in several pharmaceutical formulations. Salicylic acid (SAL), clopidogrel carboxylic acid metabolite related impurity A (CLP-RA) and clopidogrel inactiveR-enantiomer related impurity C (CLP-RC) are considered to be the main synthesis impurities and degradation products of ASP and clopidogrel. On the other hand, high efficiency and less elution are the basic requirements of high-speed chromatographic separation. So a comparative study of two simple, precise, and accurate reversed-phase HPLC-UV and UPLC-DAD methods were developed and validated for simultaneous estimation of ASP, CLP and ATV in bulk and capsules and in the presence of SAL, CLP-RA and CLP-RC. An Agilent Eclipse plus C18 (250 mm × 4.6 mm, 5 μm) for HPLC method and an Agilent Eclipse plus C18 (100 × 2.1 mm, 1.7 μm) for UPLC method were used. A gradient mobile phase for HPLC method and an isocratic mobile phase for UPLC, were used. Detection was performed for both methods at 220 nm for ASP, CLP, SAL, CLP-RA and CLP-RC, and at 240 nm for ATV. The propsed UPLC-DAD method had advantages, of being economic on the large scale with relatively much satisfactory results for sensitivity and specificity. [ABSTRACT FROM AUTHOR]