Mahrouse Marianne Alphonse, Elwy Hanan Mohamed, Salem Eman Mohamed
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini St., Cairo 11562, Egypt.
National Organization for Drug Control and Research, Giza, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2020 Nov 5;241:118647. doi: 10.1016/j.saa.2020.118647. Epub 2020 Jun 27.
Four accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of a binary mixture of cefixime (CEF) and erdosteine (ERD) without previous separation. Method A was first derivative ratio spectrophotometric method (DD) where the amplitudes at 310 and 315 nm and the amplitude at 248 nm were chosen to simultaneously estimate CEF and ERD, respectively. Method B depends on ratio difference spectrophotometry (RDSM), in which the difference in amplitudes at 325 and 326 nm on the ratio spectrum of the mixture was directly proportional to the concentration of CEF; independent of the interfering component. Similarly, the amplitude difference between 236 and 249 nm on the ratio spectrum was used for the determination of ERD. Method C was based on simultaneous determination of CEF and ERD using classical least squares (CLS) and partial least squares (PLS) chemometric techniques. Method D was the mean centering of ratio spectra (MCR) at 313 and 237 nm for the determination of CEF and ERD respectively. The developed methods were successfully employed to the determination of CEF and ERD in laboratory prepared mixtures and dosage form showing satisfactory recoveries. Methods validation was performed according to the International Conference on Harmonization (ICH) guidelines. The obtained results were statistically compared to those of the reference method, revealing no significant difference with respect to precision and accuracy. Precision and cost effectiveness of the developed methods permit their application in quality control laboratories for the determination of the binary mixture.
建立并验证了四种准确精密的分光光度法，用于不经预先分离同时测定头孢克肟（CEF）和厄多司坦（ERD）的二元混合物。方法A是一阶导数比分光光度法（DD），选择310和315 nm处的振幅以及248 nm处的振幅分别同时估算CEF和ERD。方法B基于比差分光光度法（RDSM），其中混合物比光谱上325和326 nm处的振幅差异与CEF浓度成正比；与干扰成分无关。同样，比光谱上236和249 nm之间的振幅差异用于测定ERD。方法C基于使用经典最小二乘法（CLS）和偏最小二乘法（PLS）化学计量技术同时测定CEF和ERD。方法D是分别在313和237 nm处对比光谱进行平均中心化（MCR）以测定CEF和ERD。所建立的方法成功用于测定实验室配制混合物和剂型中的CEF和ERD，回收率令人满意。根据国际协调会议（ICH）指南进行方法验证。将所得结果与参考方法的结果进行统计学比较，结果表明在精密度和准确度方面无显著差异。所建立方法的精密度和成本效益使其能够应用于质量控制实验室以测定该二元混合物。
