Abstract
A simple reversed phase high performance liquid chromatographic method with diode array detector (HPLC-DAD) has been developed and subsequently validated for the determination of fexofenadine hydrochloride (FEX) and its related compounds; keto fexofenadine (Impurity A), meta isomer of fexofenadine (Impurity B), methyl ester of fexofenadine (Impurity C) in addition to the methyl ester of ketofexofenadine (Impurity D). The separation was based on the use of a Hypersil BDS C-18 analytical column (250 × 4.6 mm, i.d., 5 μm). The mobile phase consisted of a mixture of phosphate buffer containing 0.1 gm% of 1-octane sulphonic acid sodium salt monohydrate and 1% (v/v) of triethylamine, pH 2.7 and methanol (60:40, v/v). The separation was carried out at ambient temperature with a flow rate of 1.5 ml/min. Quantitation was achieved with UV detection at 215 nm using lisinopril as internal standard, with linear calibration curves at concentration ranges 0.1-50 μg/ml for FEX and its related compounds. The optimized conditions were used to develop a stability-indicating HPLC-DAD method for the quantitative determination of FEX and its related compounds in tablet dosage forms. The drugs were subjected to oxidation, hydrolysis, photolysis and heat to apply stress conditions. Complete separation was achieved for the parent compounds and all degradation products. The method was validated according to ICH guidelines in terms of accuracy, precision, robustness, limits of detection and quantitation and other aspects of analytical validation.
Highlights
Fexofenadine, a, a-dimethyl-4-[1-hydroxy-4-[4-(hydroxydiphenyl-methyl)-1-piperidinyl] butyl]-benzene acetic acid [1] (Figure 1) is the active carboxylic acid analogue of the antihistamine terfenadine
A wavelength of 215 nm was selected for the simultaneous determination of fexofenadine hydrochloride (FEX) and its four impurities with high sensitivity
1-Octane sulphonic acid was added to the mobile phase to improve the sharpness and symmetry of FEX peaks and its related compounds
Summary
Fexofenadine, a, a-dimethyl-4-[1-hydroxy-4-[4-(hydroxydiphenyl-methyl)-1-piperidinyl] butyl]-benzene acetic acid [1] (Figure 1) is the active carboxylic acid analogue of the antihistamine terfenadine. It shares the histamine H1 receptor antagonist and non-sedative properties of the parent compound. This could be attributed to its capability to exist in zwitter-ionic form so it cannot pass through blood-brain barrier and does not cause sedation [2,3]. There are several reports on liquid chromatographic determination of FEX in biological fluids. Among which are those using LC-MS/MS [7], ultraviolet detection [8] and fluorescence detection [9]. Few methods reported the quantitation of FEX in pharmaceutical dosage forms using spectrophotometric methods [10], LC methods with ultraviolet detection [11,12,13], and capillary electrophoresis [14,15]
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