Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, El-Kasr El-Aini St, Cairo, Egypt.
Drug Test Anal. 2009 Jul;1(7):339-49. doi: 10.1002/dta.60.
In this work two well known oral hypoglycemic drugs that are administered in combination for patients with type-II diabetes were simultaneously determined. Several spectrophotometric methods were developed and validated for the determination of metformin hydrochloride (MET), pioglitazone hydrochloride (PIO) and pioglitazone acid degradate (PIO Deg). Derivative, ratio derivative, isosbestic and chemometric-assisted spectrophotometric methods were developed. The first derivative (D(1)) method was used for the determination of MET in the range of 5-30 microg x mL(-1) and PIO in the range of 10-90 microg x mL(-1) by measuring the peak amplitude at 247 nm and 280 nm, respectively. The concentration of PIO was calculated directly at 268 nm. The first derivative of ratio spectra (DD(1)) method used the peak amplitudes at 238 nm and 248.6 nm for the determination of MET in the range of 5-30 microg x mL(-1). In the isosbestic point method (ISO), the total mixture concentration was calculated by measuring the absorbance at 254.6 nm. Classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS-2) were used for the quantitative determination of MET, PIO and PIO Deg. The methods developed have the advantage of simultaneous determination of the cited components without any pre-treatment. Resolution and quantitative determination of PIO degradate with a minimum concentration of 3 microg x mL(-1) in drug samples was done. The proposed methods were successfully used to determine each drug and the acid degradate in a laboratory-prepared mixture and pharmaceutical preparations. The results were statistically compared using one-way analysis of variance (ANOVA). The methods developed were satisfactorily applied to the analysis of the two drugs in pharmaceutical formulations.
在这项工作中，同时测定了两种用于 II 型糖尿病患者的联合使用的知名口服降糖药物。开发并验证了几种分光光度法来测定盐酸二甲双胍（MET）、吡格列酮盐酸盐（PIO）和吡格列酮酸降解产物（PIO Deg）。导数、比值导数、等吸收和化学计量辅助分光光度法。一阶导数（D(1)）法用于测定 5-30μg x mL(-1)范围内的 MET 和 10-90μg x mL(-1)范围内的 PIO，分别在 247nm 和 280nm 处测量峰振幅。直接在 268nm 处计算 PIO 的浓度。比值光谱一阶导数（DD(1)）法用于测定 5-30μg x mL(-1)范围内的 MET，其峰振幅分别为 238nm 和 248.6nm。在等吸收点法（ISO）中，通过测量 254.6nm 处的吸光度来计算总混合物浓度。经典最小二乘法（CLS）、主成分回归（PCR）和偏最小二乘法（PLS-2）用于定量测定 MET、PIO 和 PIO Deg。所开发的方法具有无需任何预处理即可同时测定所引用成分的优点。在药物样品中以 3μg x mL(-1)的最小浓度成功地对 PIO 降解产物进行了分辨和定量测定。所提出的方法成功地用于实验室制备混合物和药物制剂中每种药物和酸降解产物的测定。使用单向方差分析（ANOVA）对结果进行了统计比较。所开发的方法在药物制剂中两种药物的分析中得到了满意的应用。
