Abstract
A stability-indicating micellar liquid chromatography (MLC) method was developed and validated for the assay of floctafenine (FLF) in the presence of its degradation product and main metabolite, floctafenic acid (FLA). The analysis was carried out on a CLC Shim-Pack octyl silane (C8) column (150 × 4.6 mm id, 5 μm particle size) using a micellar mobile phase consisting of 0.15 M sodium dodecyl sulfate, 10% n-propanol, and 0.3% triethylamine in 0.02 M orthophosphoric acid (pH = 3). The mobile phase was pumped at a flow rate of 1.0 mL/min with UV detection at 360 nm. The method showed good linearity for FLF and FLA over the concentration ranges of 0.5–25.0 and 0.4–10.0 μg/mL, with LODs of 0.16 and 0.12 μg/mL, respectively. The developed method was successfully applied to the determination of FLF in commercial dispersible tablets, with mean recovery of 98.87 ± 1.37%. Also, the proposed method was specific for the analysis of FLF in presence of the co-formulated drug thiocolchicoside in laboratory-prepared tablets, with mean recovery of 100.50 ± 1.07%. Statistical comparison of the results obtained by the proposed MLC method with those obtained by a comparison method showed good agreement. Moreover, the method was extended to study the degradation behavior of FLF under different International Conference on Harmonization recommended conditions such as alkaline, acidic, oxidative, thermal, and photolytic. The method was further applied for direct determination of FLA as the main metabolite of FLF in human plasma without prior extraction steps, with mean recovery of 110.50 ± 6.5%.
Determination of Putrescine and Tyramine in Fish by Micellar Liquid Chromatography with UV Detection Using Direct Injection