Maggio Rubén M, Castellano Patricia M, Vignaduzzo Silvana E, Kaufman Teodoro S
Area Análisis de Medicamentos, Facultad de Ciencias Bioquímicas y Farmacéuticas, Universidad Nacional de Rosario, Suipacha 531, Rosario S2002LRK, Argentina.
J Pharm Biomed Anal. 2007 Dec 21;45(5):804-10. doi: 10.1016/j.jpba.2007.07.024. Epub 2007 Jul 27.
An alternative method for the determination of fexofenadine (FEX) and pseudoephedrine (PSE) in their combined tablet formulation has been developed, employing the partial least squares (PLS) analysis of spectral data of the analytes in their pharmaceutical association. A full-factorially designed set of 16 synthetic samples was employed for calibration purposes. The calibration models were constructed with wavelengths selection, in the ultraviolet region, according to their predictive ability. These were validated internally by the leave-one-out procedure and externally, employing appropriate sets of validation samples. The described method was linear for both analytes, over the range 160.6-301.2 mg L(-1) for FEX (R(2)=0.9993) and between 325.6 and 610.5 mg L(-1) for PSE (R(2)=0.9992). It was accurate, exhibiting 99.8% and 99.9% drug recoveries for FEX and PSE, respectively (N=9), while in the intermediate precision experiment relative standard deviations were 1.4% for FEX and 1.2% for PSE. The contents of both analytes were assayed in commercial tablets employing this method and the results were compared with those furnished by HPLC, being in good statistical agreement. The method represents an improvement over the first derivative of spectral ratio (DSR) technique and allows high sample throughput with minimum reagent consumption and waste generation. The obtained results confirm that the method is highly suitable for its intended purpose.
已开发出一种用于测定复方片剂中非索非那定（FEX）和伪麻黄碱（PSE）的替代方法，该方法采用偏最小二乘法（PLS）分析分析物在药物组合中的光谱数据。为校准目的，使用了一组经过全因子设计的16个合成样品。根据预测能力，在紫外区域选择波长构建校准模型。这些模型通过留一法进行内部验证，并使用适当的验证样品集进行外部验证。所描述的方法对两种分析物均呈线性，FEX在160.6 - 301.2 mg L(-1)范围内（R(2)=0.9993），PSE在325.6至610.5 mg L(-1)之间（R(2)=0.9992）。该方法准确，FEX和PSE的药物回收率分别为99.8%和99.9%（N = 9），而在中间精密度实验中，FEX的相对标准偏差为1.4%，PSE为1.2%。采用该方法对市售片剂中的两种分析物含量进行了测定，并将结果与HPLC提供的结果进行比较，统计学上吻合良好。该方法相对于光谱比一阶导数（DSR）技术有所改进，可实现高样品通量，同时试剂消耗和废物产生最少。所得结果证实该方法非常适合其预期用途。
