Multivariate optimization and validation of a CZE method for the analysis of pridinol mesylate and meloxicam in tablets

Abstract

A capillary zone electrophoresis method for the simultaneous determination of pridinol mesylate (PRI) and meloxicam (MEL) employing epinastine hydrochloride and piroxicam as internal standards, was developed and optimized employing experimental design and response surface methodologies. The separation was optimally achieved in less than 2 min at 30 kV in an uncoated fused-silica capillary (41.4 cm × 75 μm I.D.), employing an 18 mmol L-1 sodium phosphate buffer solution (pH 5.90) at 25 °C. Samples were injected in hydrodynamic mode (50 mbar, 5 s) and the analytes were spectrophotometrically detected at 200 nm. Method robustness was demonstrated by ANOVA of determinations performed under conditions slightly different from the optimum. The method was validated regarding separation selectivity (peak purity factors > 0.99), linearity and range (PRI = 17.6-31.4 mg L-1; MEL = 66.5-122.5 mg L-1), accuracy (PRI = 100.2-101.9%; MEL = 98.9-100.7%) and precision. The RSD values obtained were ≥1.3% for injection repeatability and ≥1.9% for intra-day precision. The limits of detection (1.0 and 0.9 mg L-1) and quantification (3.3 and 16.5 mg L-1) of PRI and MEL, respectively, were also determined. The method was successfully applied to the determination of both drugs in three brands of tablet formulations. No statistically significant differences were observed when these results were compared with those of a RP-HPLC method.