Kinetic Spectrophotometric Analysis and Spectrofluorimetric Analysis of Ciprofloxacin Hydrochloride and Norfloxacin in Pharmaceutical Preparations Using 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-CI)

摘要

Simple, reliable, sensitive and accurate kinetic spectrophotometric and spectrofluorimetric methods were proposed for the determination of ciprofloxacin hydrochloride (CPX) and norfloxacin (NRX) in pure form and in pharmaceuticals. The methods are based on coupling the studied drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-CI) in the presence of alkaline borate buffer. Spectrophotometric measurement was achieved by recording the absorbance at 477 nm after a fixed time of 20 and 15 min on a water bath adjusted at 70 ± 1 °C for CPX and NRX, respectively. The same product exhibited emission peaks at 540 nm. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The absorbance concentration plots were linear over the ranges 3-18 and 2.5-15.0 μg/mL for CPX and NRX, respectively, while the fluorescence concentration plots were linear over the ranges 0.06-0.36 and 0.05-0.30 μg/mL for CPX and NRX, respectively. The limit of detection of the kinetic method was about 0.2 μg/mL for both drugs while the fluorescence measurement enabled their detection at a concentration of about 0.012 μg/mL. The proposed methods were successfully applied for the assay of the two drugs in their commercial products. The results obtained were statistically compared with those obtained by reference HPLC and spectrophotometric methods. The stoichiometry of the reaction was determined and the reaction pathway was postulated.