Development and validation of stability-indicating high-performance thin-layer chromatography method for estimation of ciprofibrate in bulk and in pharmaceutical formulation

Abstract

Summary A simple, selective, precise, and stability-indicating high-performance thinlayer chromatography (HPTLC) method for the analysis of ciprofibrate both in bulk drug and pharmaceutical formulation has been developed and validated. The method employed HPTLC aluminum plates precoated with silica gel 60 RP-18 F254 as the stationary phase. The solvent system consisted of methanol-water-triethylamine (2.8:2.2:0.2 υ/υ). The system was found to give compact spot for ciprofibrate (RF value of 0.55 ± 0.02). Densitometric analysis of ciprofibrate was carried out in the absorbance mode at 232 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.998 ± 0.0015 with respect to peak area in the concentration range 600–1600 ng per spot. The mean values ± SD of slope and intercept were 3.38 ± 1.47 and 986.9 ± 108.78, respectively, with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 17.84 and 54.08 ng per spot, respectively. Ciprofibrate was subjected to acid and alkali hydrolysis, oxidation, and thermal degradation. The drug undergoes degradation under acidic and basic conditions. This indicates that the drug is susceptible to acid and base. The degraded product was well resolved from the pure drug with significantly different RF value. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for the identification and quantitative determination of ciprofibrate in bulk drug and pharmaceutical formulation.