Mahmoud Ashraf M
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut 71256, Egypt.
Int J Anal Chem. 2009;2009:307045. doi: 10.1155/2009/307045. Epub 2009 Dec 2.
New rapid, sensitive, and accurate kinetic spectrophotometric methods were developed, for the first time, to determine omeprazole (OMZ) in its dosage forms. The methods were based on the formation of charge-transfer complexes with both iodine and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ). The variables that affected the reactions were carefully studied and optimized. The formed complexes and the site of interaction were examined by UV/VIS, IR, and (1)H-NMR techniques, and computational molecular modeling. Under optimum conditions, the stoichiometry of the reactions between OMZ and the acceptors was found to be 1 : 1. The order of the reactions and the specific rate constants were determined. The thermodynamics of the complexes were computed and the mechanism of the reactions was postulated. The initial rate and fixed time methods were utilized for the determination of OMZ concentrations. The linear ranges for the proposed methods were 0.10-3.00 and 0.50-25.00 mug mL(-1) with the lowest LOD of 0.03 and 0.14 mug mL(-1) for iodine and DDQ, respectively. Analytical performance of the methods was statistically validated; RSD was <1.25% for the precision and <1.95% for the accuracy. The proposed methods were successfully applied to the analysis of OMZ in its dosage forms; the recovery was 98.91-100.32% +/- 0.94-1.84, and was found to be comparable with that of reference method.
首次开发了快速、灵敏且准确的动力学分光光度法,用于测定剂型中的奥美拉唑(OMZ)。这些方法基于与碘和2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)形成电荷转移络合物。仔细研究并优化了影响反应的变量。通过紫外/可见光谱、红外光谱和(1)H-核磁共振技术以及计算分子建模对形成的络合物和相互作用位点进行了研究。在最佳条件下,发现OMZ与受体之间反应的化学计量比为1:1。确定了反应级数和比速率常数。计算了络合物的热力学并推测了反应机理。采用初始速率法和固定时间法测定OMZ浓度。所提出方法的线性范围分别为0.10 - 3.00和0.50 - 25.00 μg mL(-1),碘和DDQ的最低检测限分别为0.03和0.14 μg mL(-1)。对方法的分析性能进行了统计学验证;精密度的相对标准偏差(RSD)<1.25%,准确度的RSD<1.95%。所提出的方法成功应用于剂型中OMZ的分析;回收率为98.91 - 100.32% ± 0.94 - 1.84,发现与参考方法相当。