title: Validated column high-performance liquid chromatographic method for determination of aspirin and clopidogrel in combined tablets in the presence of degradation products formed under ICH-recommended stress conditions.
abstract: The development and validation of a column high-performance liquid chromatographic assay method for the determination of aspirin and clopidogrel in tablet formulation are described. The combination formulation was subjected to International Conference on Harmonization-recommended stress conditions. Separation of the drugs from the degradation products formed under stress conditions was achieved on an octasilyl (C8) column using 0.3% orthophosphoric acid-acetonitrile (65 + 35, v/v) mobile phase. The method was validated for specificity, linearity, limits of detection and quantification, precision, accuracy, and robustness. The method was found to be specific against placebo interference and during the forced degradation. The response was linear in the concentration range of 30.0-120.0 microg/mL for aspirin and 15.0-60.0 microg/mL for clopidogrel, with a correlation coefficient of 0.9999 for both. The relative standard deviation values for intra- and interday precision were <2.0%. The accuracy was between 99.12 and 99.83% for aspirin and 98.20 and 100.35% for clopidogrel. Stress testing showed degradation products that were well-separated from the parent compound, confirming the stability-indicating capacity of the method.
authors.affiliation: Saurashtra University, Department of Chemistry, Rajkot-360 005, Gujarat, India.
authors.forename: Pankaj K
authors.initials: PK
authors.lastname: Kachhadia
authors.forename: Ashish S
authors.initials: AS
authors.lastname: Doshi
authors.forename: Hitendra S
authors.initials: HS
authors.lastname: Joshi
mesh_terms: D001241:Aspirin / Q000032:analysis* / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D000077144:Clopidogrel; D006863:Hydrogen-Ion Concentration; D010975:Platelet Aggregation Inhibitors / Q000032:analysis / Q000302:isolation & purification; D015203:Reproducibility of Results; D013314:Stress, Mechanical; D013607:Tablets / Q000032:analysis* / Q000737:chemistry*; D013988:Ticlopidine / Q000031:analogs & derivatives* / Q000032:analysis / Q000302:isolation & purification
chemical_list: D010975:Platelet Aggregation Inhibitors; D013607:Tablets; D000077144:Clopidogrel; D013988:Ticlopidine; D001241:Aspirin