Assay Method for Quality Control and Stability Studies of a New Antithrombotic Agent (S007-867)

摘要

A substituted 5-(piperidine-1-carbonyl) pyrrolidin-2-one (CDRI compound S007-867) is a potent antithrombotic candidate drug under development at our Institute. An HPLC method for determination of S007-867 with its intermediates has been developed and validated for in process quality control and stability studies. The analytical performance parameters such as specificity, limit of detection (LOD), lower limit of quantification (LLOQ), linearity, precision, robustness, and accuracy were determined according to International Conference on Harmonization ICH Q2(R1) guidelines. HPLC separation was achieved on C18 Lichrospheres column (250 mm, 4 mm, 5 mu m, Merck) using water containing 0.1% glacial acetic acid and acetonitrile as the mobile phase in an isocratic elution. The eluents were monitored by a photo diode array detector at 220 nm. Based on signal to noise ratio of 3 and 10 the LOD of S007-867 was 0.98 mu g/mL, while the LLOQ was 3.9 mu g/mL. The calibration curves were linear in the range of 3.97125 mu g/mL. Precision of the method was determined by inter- and intra-assay variations within the range.