Acta Pharm. 2014 Mar;64(1):63-75. doi: 10.2478/acph-2014-0008.
The study describes the development and validation of a new microwell-based spectrophotometric assay for determination of olmesartan medoxomil (OLM) in tablets. The formation of a colored charge-transfer (CT) complex between OLM as an n-electron donor and 2,3-dichloro- -5,6-dicyano-1,4-benzoquinone (DDQ) as a p-electron acceptor was investigated, and employed as the basis for the development of the new assay. The proposed assay was conducted in 96-microwell plates. The absorbance of the colored-CT complex was measured at 460 nm with a microplate reader. Optimum conditions of the reaction and the analytical procedures of the assay were established. Under the optimum conditions, a linear relationship with a good correlation coefficient was found between the absorbance and the concentration of OLM in the range of 2-200 μg per well. The limits of detection and quantitation were 0.53 and 1.61 μg per well, respectively. No interference was observed from the excipients present in OLM tablets or from hydrochlorothiazide and amlodipine besylate that were co-formulated with OLM in some of its formulations. The assay was successfully applied to the analysis of OLM in tablets with good accuracy and precision. The assay described herein has a great practical value in the routine analysis of OLM in quality control laboratories, since it has a high throughput property and consumes low volumes of organic solvent. It thus offers a reduction in the exposure of analysts to the toxic effects of organic solvents, as well as a reduction in the cost of analysis.
本研究描述了一种新的微孔板分光光度测定法的开发和验证,用于测定片剂中的奥美沙坦酯(OLM)。研究了 OLM 作为 n-电子供体与 2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)作为 p-电子受体之间形成的有色电荷转移(CT)复合物,并将其用作新测定法的基础。该新测定法在 96 微孔板中进行。用微孔板读数器在 460nm 处测量有色 CT 复合物的吸光度。确定了反应的最佳条件和分析程序。在最佳条件下,在每个孔 2-200μg 的范围内,吸光度与 OLM 浓度之间存在线性关系,相关系数良好。检测限和定量限分别为 0.53 和 1.61μg/孔。在 OLM 片剂中的赋形剂或与 OLM 共同配制的氢氯噻嗪和苯磺酸氨氯地平存在的情况下,没有观察到干扰。该测定法成功地应用于 OLM 片剂的分析,具有良好的准确性和精密度。该测定法在质量控制实验室中对 OLM 的常规分析具有重要的实用价值,因为它具有高通量的特性,并且有机溶剂的用量低。因此,它减少了分析人员接触有机溶剂毒性作用的机会,并降低了分析成本。