Askal Hassan F, Refaat Ibrahim H, Darwish Ibrahim A, Marzouq Mostafa A
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2008 Apr;69(4):1287-91. doi: 10.1016/j.saa.2007.07.031. Epub 2007 Jul 31.
A selective spectrophotometric method for the determination of rosoxacin (ROS), a 4-quinolone antimicrobial agent, has been developed and validated. The method was based on the reaction of ROS with alkaline sodium nitroprusside (SNP) reagent at room temperature forming a red colored chromogen measured at 455 nm. The conditions affecting the reaction (SNP concentration, pH, color-developing time, temperature, diluting solvent and chromogen stability time) were optimized. Under the optimum conditions, good linear relationship (r=0.9987) was obtained between the absorbance and the concentration of ROS in the range of 20-50 microg ml(-1). The assay limits of detection and quantitation were 2.5 and 8.4 microg ml(-1), respectively. The method was successfully applied to the analysis of bulk drug and laboratory-prepared tablets; the mean percentage recoveries were 100.1+/-0.33 and 101.24+/-1.28%, respectively. The results were compared favourably with those obtained by the reported method; no significant difference in the accuracy and precision as revealed by the accepted values of t- and F-tests, respectively. The robustness and ruggedness of the method was checked and satisfactory results were obtained. The proposed method was found to be highly selective for ROS among the fluoroquinolone antibiotics. The reaction mechanism was proposed and it proceeded in two steps; the formation of nitroferrocyanide by the action of sodium hydroxide alkalinity on SNP and the subsequent formation of the colored nitrosyl-ROS derivative by the attack at position 6 of ROS.
已开发并验证了一种用于测定4-喹诺酮类抗菌剂罗索沙星(ROS)的选择性分光光度法。该方法基于ROS与碱性硝普钠(SNP)试剂在室温下反应,形成在455nm处测定的红色显色剂。优化了影响反应的条件(SNP浓度、pH值、显色时间、温度、稀释溶剂和显色剂稳定性时间)。在最佳条件下,ROS浓度在20 - 50μg ml⁻¹范围内时,吸光度与ROS浓度之间呈现良好的线性关系(r = 0.9987)。检测限和定量限分别为2.5和8.4μg ml⁻¹。该方法成功应用于原料药和实验室制备片剂的分析;平均回收率分别为100.1±0.33%和101.24±1.28%。将结果与报道方法获得的结果进行比较,t检验和F检验的公认值分别表明在准确性和精密度方面无显著差异。检查了该方法的稳健性和耐用性,获得了满意的结果。发现所提出的方法对氟喹诺酮类抗生素中的ROS具有高度选择性。提出了反应机理,该反应分两步进行;氢氧化钠碱度作用于SNP形成亚铁氰化硝基,随后ROS的6位受到攻击形成有色亚硝基-ROS衍生物。