title: Evaluation of N-bromosuccinimide as a new analytical reagent for the spectrophotometric determination of fluoroquinolone antibiotics.
abstract: Analytical studies were carried out, for the first time, to evaluate the use of N-bromosuccinimide (NBS) as an analytical reagent for the spectrophotometric determination of eleven therapeutically important fluoroquinolone antibiotics (FQA). The procedures involved the reaction of the FQA with NBS and subsequent measurement of the excess NBS by its reaction with p-phenylenediamine (PDA) to give a violet colored product that was measured at 530 nm. Different variables affecting the reaction (concentration of NBS, concentration of PDA, pH of reaction medium, reaction time, and the diluting solvents) were carefully studied and optimized. The molar ratio and mechanism of the reaction between each of the studied FQA with NBS were proposed using UV-vis, IR, and NMR techniques. Under the optimum reaction conditions, the analytical method was developed and validated. Beer's law was obeyed in the general concentration range of 3-25 microg/ml. The assay limits of detection and quantitation were 0.33-1.29 and 1.10-4.31 microg/ml, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2%. The proposed method was successfully applied to the analysis of the investigated FQA in their pure and pharmaceutical dosage forms without interference from the common excipients (label claim values were 99.85-100.17+/-0.13-0.59%). Interference from ascorbic acid, that is co-formulated as a stabilizer for the ampoule form, was avoided by its pre-oxidation with potassium bromate before applying the analytical procedure. The results obtained by the proposed method were comparable with those obtained by the official and reported methods.
authors.affiliation: Department of Pharmaceutical Analytical Chemistry, Assiut University, Assiut 71526, Egypt.
authors.forename: Hassan
authors.initials: H
authors.lastname: Askal
authors.forename: Ibrahim
authors.initials: I
authors.lastname: Refaat
authors.forename: Ibrahim
authors.initials: I
authors.lastname: Darwish
authors.forename: Mostafa
authors.initials: M
authors.lastname: Marzouq
mesh_terms: D000900:Anti-Bacterial Agents / Q000032:analysis*; D001205:Ascorbic Acid / Q000737:chemistry; D001959:Bromates / Q000737:chemistry; D001974:Bromosuccinimide / Q000737:chemistry*; D024841:Fluoroquinolones / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D009682:Magnetic Resonance Spectroscopy; D015394:Molecular Structure; D010084:Oxidation-Reduction; D015203:Reproducibility of Results; D013997:Time Factors
chemical_list: D000900:Anti-Bacterial Agents; D001959:Bromates; D024841:Fluoroquinolones; C019536:potassium bromate; D001974:Bromosuccinimide; D001205:Ascorbic Acid