Thesis (M.Sc.) - Cairo University - Faculty of Science - Department of Analytical Chemistry

A simple, precise, specific and accurate reversed phase HPLC (RP-HPLC) method has been developed for the determination of solifenacin succinate (SOLS), flavoxate HCl (FLXHC) and toltoridine tartarate (TOLT) in bulk and in pharmaceutical dosage forms. The proposed RP-HPLC method was carried out using Xterra RP-18 column (5 om practical size, 25 cmx4.6 mm i.d.). The flow rate, the injection volume and the detection wavelength were 1.0 mL/min, 20 mL and 200 nm, respectively. The mobile phase consisted of 0.05 M pentane sulfonic acid sodium salt (SOLS: pH 3.0±0.05, FLXHC and TOLT: pH 5.5±0.05) and acetonitrile (50:50 v/v). The retention times for SOLS, FLXHC and TOLT drugs were found to be 4.08±0.06, 4.30±0.03 and 5.85±0.07 min, respectively. The calibration was linear over the concentration range of 0.1-100 ogmL-1. The mean recoveries for SOLS, FLXHC and TOLT drugs were about 99.80, 100.43 and 100.00%, respectively. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. In this work SOLS, FLXHC and TOLT drugs were investigated using thermal analysis (TA) measurements (TG-DTA) in comparison with electron impact (EI) mass spectral (MS) fragmentation at 70 eV. Also determination of chemical purity, melting range using differential scanning calorimetry (DSC), and variation of enthalpy in the process of characterizing medicines is one of the principal requirements evaluated in quality control of the pharmaceutical industry

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