Hegazy Maha Abdel-Monem, Eissa Maya Shaaban, Abd El-Sattar Osama Ibrahim, Abd El-Kawy Mohamed Mohamed
Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo, Egypt.
Analytical Chemistry Department, Faculty of Pharmacy, Egyptian Russian University, Cairo, Egypt.
J Pharm Anal. 2014 Apr;4(2):132-143. doi: 10.1016/j.jpha.2013.09.006. Epub 2013 Oct 8.
Simple, accurate, sensitive and validated UV spectrophotometric and chemometric methods were developed for the determination of imidapril hydrochloride (IMD) in the presence of both its alkaline (AKN) and oxidative (OXI) degradation products and in its pharmaceutical formulation. Method A is the fourth derivative spectra (D4) which allows the determination of IMD in the presence of both AKN and OXD, in pure form and in tablets by measuring the peak amplitude at 243.0 nm. Methods B, C and D, manipulating ratio spectra, were also developed. Method B is the double divisor-ratio difference spectrophotometric one (DD-RD) by computing the difference between the amplitudes of IMD ratio spectra at 232 and 256.3 nm. Method C is the double divisor-first derivative of ratio spectra method (DD-DR1) at 243.2 nm, while method D is the mean centering of ratio spectra (MCR) at 288.0 nm. Methods A, B, C and D could successfully determine IMD in a concentration range of 4.0-32.0 µg/mL. Methods E and F are principal component regression (PCR) and partial least-squares (PLS), respectively, for the simultaneous determination of IMD in the presence of both AKN and OXI, in pure form and in its tablets. The developed methods have the advantage of simultaneous determination of the cited components without any pre-treatment. The accuracy, precision and linearity ranges of the developed methods were determined. The results obtained were statistically compared with those of a reported HPLC method, and there was no significant difference between the proposed methods and the reported method regarding both accuracy and precision.
开发了简单、准确、灵敏且经过验证的紫外分光光度法和化学计量学方法，用于在存在碱性（AKN）和氧化（OXI）降解产物的情况下以及在其药物制剂中测定盐酸咪达普利（IMD）。方法A是四阶导数光谱（D4），通过测量243.0 nm处的峰高，可在纯形式和片剂中同时测定存在AKN和OXD时的IMD。还开发了方法B、C和D，它们通过处理比率光谱来测定。方法B是双除数比率差分光光度法（DD-RD），通过计算IMD比率光谱在232和256.3 nm处的振幅差来测定。方法C是比率光谱的双除数一阶导数法（DD-DR1），在243.2 nm处测定，而方法D是比率光谱的平均中心化法（MCR），在288.0 nm处测定。方法A、B、C和D能够成功测定浓度范围为4.0 - 32.0 μg/mL的IMD。方法E和F分别是主成分回归（PCR）和偏最小二乘法（PLS），用于在存在AKN和OXI的情况下同时测定纯形式及其片剂中的IMD。所开发的方法具有无需任何预处理即可同时测定上述成分的优点。测定了所开发方法的准确度、精密度和线性范围。将所得结果与报道的高效液相色谱法的结果进行统计学比较，所提出的方法与报道方法在准确度和精密度方面均无显著差异。
