Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, Riyadh, Saudi Arabia.
Spectrochim Acta A Mol Biomol Spectrosc. 2010 Jan;75(1):334-9. doi: 10.1016/j.saa.2009.10.036. Epub 2009 Oct 31.
A selective and simple kinetic spectrophotometric has been developed, for the first time, for the determination of gatifloxacin (GAT) in its dosage forms. The method was based on the formation of a colored N-vinyl chlorobenzoquinone derivative of GAT by its reaction with 2,3,5,6-tetrachloro-1,4-benzoquinone in presence of acetaldehyde. The formation of the colored product was monitored spectrophotometrically by measuring the absorbances at 655 nm. The factors affecting the reaction were studied and optimized. The stoichiometry of the reaction was determined, and the reaction pathway was postulated. Under the optimized conditions, the initial rate and fixed time (at 5 min) methods were utilized for constructing the calibration graphs. The graphs were linear in the concentration ranges of 2-100 and 10-140 microg ml(-1) with limits of detection of 0.84 and 3.5 microg ml(-1) for the initial rate and fixed time methods, respectively. The analytical performance of both methods was fully validated, and the results were satisfactory. The proposed methods were successfully applied to the determination of GAT in its commercial dosage forms. The label claim percentages were 99.7-100.5 and 98.2-99.5% for the initial rate and fixed time methods, respectively. Statistical comparison of the results with those of the reference method showed excellent agreement and proved that there was no significant difference in the accuracy and precision between the reference and the proposed methods. The proposed methods are superior to all the previously reported spectrophotometric methods in terms of the procedure simplicity and assay selectivity.
一种选择性和简单的动力学分光光度法首次被开发出来,用于测定其制剂中的加替沙星(GAT)。该方法基于 GAT 与 2,3,5,6-四氯-1,4-苯醌在乙醛存在下反应形成有色 N-乙烯基氯苯醌衍生物。通过在 655nm 处测量吸光度来监测有色产物的形成。研究并优化了影响反应的因素。确定了反应的化学计量比,并提出了反应途径。在优化条件下,采用初始速率法和固定时间法(在 5 分钟时)构建校准曲线。在 2-100 和 10-140μgml(-1)浓度范围内,初始速率和固定时间法的线性范围分别为 2-100 和 10-140μgml(-1),检测限分别为 0.84 和 3.5μgml(-1)。两种方法的分析性能均得到充分验证,结果令人满意。该方法成功应用于其商业制剂中 GAT 的测定。初始速率法和固定时间法的标签声称百分率分别为 99.7-100.5%和 98.2-99.5%。与参考方法相比,结果的统计比较表明,两种方法的准确性和精密度之间没有显著差异。与之前报道的所有分光光度法相比,该方法在程序简单性和分析选择性方面具有优越性。