Three simple and rapid spectrophotometric methods were developed for detection and trace determination of benzophenone (the main impurity) in phenytoin bulk powder and pharmaceutical formulations. The first method, zero-crossing first derivative spectrophotometry, depends on measuring the first derivative trough values at 257.6 nm for benzophenone. The second method, zero-crossing third derivative spectrophotometry, depends on measuring the third derivative peak values at 263.2 nm. The third method, ratio first derivative spectrophotometry, depends on measuring the peak amplitudes of the first derivative of the ratio spectra (the spectra of benzophenone divided by the spectrum of 5.0 μg/mL phenytoin solution) at 272 nm. The calibration graphs were linear over the range of 1-10 μg/mL. The detection limits of the first and the third derivative methods were found to be 0.04 μg/mL and 0.11 μg/mL and the quantitation limits were 0.13 μg/mL and 0.34 μg/mL, respectively, while for the ratio derivative method, the detection limit was 0.06 μg/mL and the quantitation limit was 0.18 μg/mL. The proposed methods were applied successfully to the assay of the studied drug in phenytoin bulk powder and certain pharmaceutical preparations. The results were statistically compared to those obtained using a polarographic method and were found to be in good agreement.
A derivative UV-spectrophotometric analytical procedure was developed for determination of three 4-quinolone antibacterials: norfloxacin (NFX), ciprofloxacin (CFX), and sparfloxacin (SFX). The method depends on the complexation of Cu(II) with the studied compounds in aqueous medium. A third order, measurement was applied for their quantification. A linear correlation was established between the amplitude of the peak and concentration for all the studied drugs in the range of 15–80, 35–120, and 200–700 ng/mL, with minimum detectability (S/N = 2) of 1.0, 1.3, and 5.1 ng/mL for NFX, CFX, and SFX, respectively. The method was successfully applied for accurate, sensitive, and selective determination of the studied drugs in bulk and tablets formulation with average percentage recoveries of 99.22 ± 0.55 to 100.33 ± 1.60. The results obtained were favorably compared with those of the reference method. The method was also used to determine sparfloxacin in spiked human plasma and urine. The results obtained were satisfactory, accurate, and precise.
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