Aydoğmuş Zeynep
Department of Analytical Chemistry, Faculty of Pharmacy, Istanbul University, 34116 Beyazit, Istanbul, Turkey.
Spectrochim Acta A Mol Biomol Spectrosc. 2008 Jun;70(1):69-78. doi: 10.1016/j.saa.2007.07.012. Epub 2007 Jul 17.
Three sensitive, selective, accurate spectrophotometric and spectrofluorimetric methods have been developed for the determination of ropinirole hydrochloride in tablets. The first method was based on measuring the absorbance of drug solution in methanol at 250 nm. The Beer's law was obeyed in the concentration range 2.5-24 microg ml(-1). The second method was based on the charge transfer reaction of drug, as n-electron donor with 7,7,8,8-tetracyanoquinodimethane (TCNQ), as pi-acceptor in acetonitrile to give radical anions that are measured at 842 nm. The Beer's law was obeyed in the concentration range 0.6-8 microg ml(-1). The third method was based on derivatization reaction with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer of pH 8.5 followed by measuring the fluorescence intensity at 525 nm with excitation at 464 nm in chloroform. Beer's law was obeyed in the concentration range 0.01-1.3 microg ml(-1). The derivatization reaction product of drug with NBD-Cl was characterized by IR, 1H NMR and mass spectroscopy. The developed methods were validated. The following analytical parameters were investigated: the molar absorptivity (epsilon), limit of detection (LOD, microg ml(-1)) and limit of quantitation (LOQ, microg ml(-1)), precision, accuracy, recovery, and Sandell's sensitivity. Selectivity was validated by subjecting stock solution of ropinirole to acidic, basic, oxidative, and thermal degradation. No interference was observed from common excipients present in formulations. The proposed methods were successfully applied for determination of drug in tablets. The results of these proposed methods were compared with each other statistically.
已开发出三种灵敏、选择性好、准确的分光光度法和荧光分光光度法用于测定片剂中的盐酸罗匹尼罗。第一种方法是基于测量药物溶液在甲醇中250 nm处的吸光度。在2.5 - 24 μg ml⁻¹的浓度范围内符合比尔定律。第二种方法基于药物作为n电子供体与7,7,8,8 - 四氰基对苯二醌二甲烷(TCNQ)作为π受体在乙腈中的电荷转移反应,生成在842 nm处测量的自由基阴离子。在0.6 - 8 μg ml⁻¹的浓度范围内符合比尔定律。第三种方法基于在pH 8.5的硼酸盐缓冲液中与4 - 氯 - 7 - 硝基苯并呋咱(NBD - Cl)的衍生化反应,然后在氯仿中于464 nm激发下测量525 nm处的荧光强度。在0.01 - 1.3 μg ml⁻¹的浓度范围内符合比尔定律。药物与NBD - Cl的衍生化反应产物通过红外光谱、¹H核磁共振和质谱进行了表征。所开发的方法经过了验证。研究了以下分析参数:摩尔吸光系数(ε)、检测限(LOD,μg ml⁻¹)和定量限(LOQ,μg ml⁻¹)、精密度、准确度、回收率和桑德尔灵敏度。通过使罗匹尼罗储备溶液经受酸性、碱性、氧化和热降解来验证选择性。未观察到制剂中常见辅料的干扰。所提出的方法成功应用于片剂中药物的测定。对这些所提出方法的结果进行了统计学比较。