Abdel Hameed Eman A, Abdel Salam Randa A, Hadad Ghada M
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Suez Canal University, Ismailia 41522, Egypt.
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Suez Canal University, Ismailia 41522, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2015 Apr 15;141:278-86. doi: 10.1016/j.saa.2015.01.035. Epub 2015 Jan 30.
Chemometric-assisted spectrophotometric methods and high performance liquid chromatography (HPLC) were developed for the simultaneous determination of the seven most commonly prescribed β-blockers (atenolol, sotalol, metoprolol, bisoprolol, propranolol, carvedilol and nebivolol). Principal component regression PCR, partial least square PLS and PLS with previous wavelength selection by genetic algorithm (GA-PLS) were used for chemometric analysis of spectral data of these drugs. The compositions of the mixtures used in the calibration set were varied to cover the linearity ranges 0.7-10 μg ml(-1) for AT, 1-15 μg ml(-1) for ST, 1-15 μg ml(-1) for MT, 0.3-5 μg ml(-1) for BS, 0.1-3 μg ml(-1) for PR, 0.1-3 μg ml(-1) for CV and 0.7-5 μg ml(-1) for NB. The analytical performances of these chemometric methods were characterized by relative prediction errors and were compared with each other. GA-PLS showed superiority over the other applied multivariate methods due to the wavelength selection. A new gradient HPLC method had been developed using statistical experimental design. Optimum conditions of separation were determined with the aid of central composite design. The developed HPLC method was found to be linear in the range of 0.2-20 μg ml(-1) for AT, 0.2-20 μg ml(-1) for ST, 0.1-15 μg ml(-1) for MT, 0.1-15 μg ml(-1) for BS, 0.1-13 μg ml(-1) for PR, 0.1-13 μg ml(-1) for CV and 0.4-20 μg ml(-1) for NB. No significant difference between the results of the proposed GA-PLS and HPLC methods with respect to accuracy and precision. The proposed analytical methods did not show any interference of the excipients when applied to pharmaceutical products.
已开发出化学计量学辅助分光光度法和高效液相色谱法(HPLC),用于同时测定七种最常用的β受体阻滞剂(阿替洛尔、索他洛尔、美托洛尔、比索洛尔、普萘洛尔、卡维地洛和奈必洛尔)。主成分回归(PCR)、偏最小二乘法(PLS)以及通过遗传算法进行波长选择的偏最小二乘法(GA-PLS)用于这些药物光谱数据的化学计量学分析。校准集中使用的混合物组成有所变化,以覆盖阿替洛尔(AT)0.7 - 10 μg ml⁻¹、索他洛尔(ST)1 - 15 μg ml⁻¹、美托洛尔(MT)1 - 15 μg ml⁻¹、比索洛尔(BS)0.3 - 5 μg ml⁻¹、普萘洛尔(PR)0.1 - 3 μg ml⁻¹、卡维地洛(CV)0.1 - 3 μg ml⁻¹和奈必洛尔(NB)0.7 - 5 μg ml⁻¹的线性范围。这些化学计量学方法的分析性能通过相对预测误差来表征,并相互比较。由于波长选择,GA-PLS显示出优于其他应用的多元方法。使用统计实验设计开发了一种新的梯度HPLC方法。借助中心复合设计确定了最佳分离条件。所开发的HPLC方法在阿替洛尔0.2 - 20 μg ml⁻¹、索他洛尔0.2 - 20 μg ml⁻¹、美托洛尔0.1 - 15 μg ml⁻¹、比索洛尔0.1 - 15 μg ml⁻¹、普萘洛尔0.1 - 13 μg ml⁻¹、卡维地洛0.1 - 13 μg ml⁻¹和奈必洛尔0.4 - 20 μg ml⁻¹范围内呈线性。所提出的GA-PLS方法和HPLC方法在准确度和精密度方面的结果无显著差异。所提出的分析方法应用于药品时未显示出任何辅料干扰。