Solid dispersions were prepared via a solvent evaporation method, employing ethanol\n(96%, v/v) as solvent, with three different polymers as carrier: povidone, copovidone, and poloxamer\n407. Previously developed reversed-phase HPLC (RP-HPLC) methods were modified and used for\nthe simultaneous determination of acetylsalicylic acid and clopidogrel bisulfate and after release\nfrom solid dispersions. Chromatography was carried out on a C-18 column, with a mobile phase of\nacetonitrileâ??methanolâ??phosphate buffer pH 3.0, UV detection at 240 nm, and a run time of 6 min.\nThe method was validated according to International Conference of Harmonisation guidelines and\nvalidation included specificity, accuracy, precision, linearity, robustness, limit of detection (LOD),\nand limit of quantification (LOQ). The method is specific for determination of acetylsalicylic acid and\nclopidogrel bisulfate. The linearity was provided in the concentration range 0.0275â??0.1375 mg/mL\nfor acetylsalicylic acid and 0.0200â??0.1000 mg/mL for clopidogrel bisulfate, with a correlation\ncoeffcient (R2 value) of 0.9999 for both active pharmaceutical ingredients (APIs). Accuracy was\nconfirmed by calculated recoveries for acetylsalicylic acid (98.6â??101.0%) and clopidogrel bisulfate\n(100.0â??101.6%). The intra-day and the inter-day precision-calculated relative standard deviations\nare less than 1%, which indicates high precision of the method. The limits of detection and\nquantification for acetylsalicylic acid were 0.0004 and 0.0012 mg/mL, and for clopidogrel bisulfate\n0.0002 mg/mL and 0.0007 mg/mL, respectively. Small variations in chromatographic conditions did\nnot significantly affect qualitative and quantitative system responses, which proved robustness of\nmethod. The proposed RP-HPLC method was applied for simultaneous determination of clopidogrel\nbisulfate and acetylsalicylic acid from solid dispersions.
Loading....