Ibrahim F, Wahba M E K
Department of Analytical Chemistry Faculty of Pharmacy, Mansoura University, Mansoura, 35516, Egypt.
J Fluoresc. 2014 Jul;24(4):1137-47. doi: 10.1007/s10895-014-1394-z. Epub 2014 Jun 3.
Two simple, sensitive, rapid, economic and validated methods, namely reversed phase liquid chromatography (method Ι) and third derivative synchronous fluorescence spectroscopy (method ΙΙ) have been developed for the simultaneous determination of rabeprazole sodium and domperidone in their laboratory prepared mixture after derivatization with 4-Chloro-7-nitrobenzofurazan. Reversed phase chromatography was conducted using a Zorbax® SB-Phenyl column (250.0 mm × 4.6 mm id) combined with a guard column at ambient temperature with fluorimetric detection at 540 nm after excitation at 483 nm. A mobile phase composed of a mixture of distilled water with methanol and acetonitrile in a ratio of 50:20:30 adjusted pH to 4 has been used at a flow rate of 1 mL/min. Sharp well resolved peaks were obtained for domperidone and rabeprazole sodium with retention times of 5.5 and 6.4 min respectively. While in method ΙΙ, the third-derivative spectra were estimated at 507 and 436 nm for rabeprazole sodium and domperidone respectively. Linearity ranges for rabeprazole sodium and domperidone respectively in both methods were found to be 0.15-2.0 and 0.1-1.5 μg/mL. The proposed methods were successfully applied for the analysis of the two compounds in their binary mixtures, and laboratory prepared tablets. The obtained results were favorably compared with those obtained by the comparison method. Furthermore, detailed validation procedure was also conducted.
已开发出两种简单、灵敏、快速、经济且经过验证的方法,即反相液相色谱法(方法Ⅰ)和三阶导数同步荧光光谱法(方法Ⅱ),用于在与4-氯-7-硝基苯并呋咱衍生化后,同时测定实验室制备混合物中的雷贝拉唑钠和多潘立酮。反相色谱使用Zorbax® SB-苯基柱(250.0 mm×4.6 mm内径)结合保护柱,在室温下进行,在483 nm激发后于540 nm处进行荧光检测。流动相由蒸馏水与甲醇和乙腈按50:20:30比例混合而成,并将pH值调至4,流速为1 mL/min。多潘立酮和雷贝拉唑钠获得尖锐且分离良好的峰,保留时间分别为5.5和6.4分钟。而在方法Ⅱ中,雷贝拉唑钠和多潘立酮的三阶导数光谱分别在507和436 nm处测定。两种方法中雷贝拉唑钠和多潘立酮的线性范围分别为0.15 - 2.0和0.1 - 1.5 μg/mL。所提出的方法成功应用于分析二元混合物及实验室制备片剂中的这两种化合物。将所得结果与比较法所得结果进行了良好比较。此外,还进行了详细的验证程序。