Radhakrishna T, Om Reddy G
Department of Analytical Research, Dr. Reddy's Research Foundation, Miyapur, 500 050, Hyderabad, India.
J Pharm Biomed Anal. 2002 Jul 20;29(4):681-90. doi: 10.1016/s0731-7085(02)00181-4.
A simple reversed phase liquid chromatographic (RPLC) method has been developed and subsequently validated for the determination of fexofenadine hydrochloride and its related compounds A and B. The method utilizes a C8 column for the separation and determination of meta-isomer (related compound B). The separation was achieved using an Eclipse XDB C8, 5 microm, 4.6 x 150 mm column and a mobile phase comprising 1% triethylamine phosphate (pH 3.7), acetonitrile and methanol in the ratio 60:20:20 (v/v/v). 5-Methyl 2-nitrophenol has been used as internal standard for the purpose of quantitation of fexofenadine. The described method was linear over a range of 0.7-18.7 microg/ml for related compounds A and B and 60-750 microg/ml for assay of fexofenadine. The relative standard deviation (n=3) was 0.5% for the drug and 3.4% for related compounds. The intermediate precision was 0.79% (n=9) for assay and 5.16% (n=9) for related impurities. The mean recovery of both the related compounds were in the range of 94-103%. Limits of detection (LOD) and quantification (LOQ) for the related compounds A and B were 0.18, 0.12 and 0.56, 0.48 microg/ml, respectively. The precision of the method was checked by F-test using a reported method as reference and the calculated value (1.35) was found to be less than the table value at 95% confidence levels. The obtained results confirm that the method is highly suitable for its intended purpose.
已开发出一种简单的反相液相色谱（RPLC）方法，并随后对其进行了验证，用于测定盐酸非索非那定及其相关化合物A和B。该方法使用C8柱分离并测定间位异构体（相关化合物B）。分离采用Eclipse XDB C8，5微米，4.6×150毫米柱，流动相由1%磷酸三乙胺（pH 3.7）、乙腈和甲醇按60:20:20（v/v/v）的比例组成。5-甲基-2-硝基苯酚用作内标，用于定量非索非那定。所描述的方法在0.7 - 18.7微克/毫升范围内对相关化合物A和B呈线性，在60 - 750微克/毫升范围内对非索非那定的含量测定呈线性。该药物的相对标准偏差（n = 3）为0.5%，相关化合物的相对标准偏差为3.4%。含量测定的中间精密度为0.79%（n = 9），相关杂质的中间精密度为5.16%（n = 9）。两种相关化合物的平均回收率在94 - 103%范围内。相关化合物A和B的检测限（LOD）和定量限（LOQ）分别为0.18、0.12和0.56、0.48微克/毫升。使用一种报道的方法作为参考，通过F检验检查了该方法的精密度，发现在95%置信水平下计算值（1.35）小于表值。所得结果证实该方法非常适合其预期用途。
