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Development of a thin-layer chromatographic method for the enantioresolution of sotalol using levofloxacin as chiral selector
JPC - Journal of Planar Chromatography - Modern TLC ( IF 1.6 ) Pub Date : 2021-01-07 , DOI: 10.1007/s00764-020-00068-3
Vinod Kumar Vashistha , Anuj Kumar

In this work, a commercially available, chirally pure pharmaceutical containing carboxylic group, namely, levofloxacin was utilized as chiral selector for the enantioresolution of sotalol. The TLC plates were prepared by mixing levofloxacin in silica gel slurry. The racemic mixture of sotalol was applied on TLC plates using MeCN–MeOH–H2O (5.2:2.0:0.8, V/V; pH = 5.0) as the mobile phase at 22 (± 2) °C. The separation conditions were optimized in terms of concentration of chiral selector, pH, and temperature to get successful separation. The resolution value was observed to be 2.6. The enantiomers so separated were isolated from TLC plates and characterized using various techniques. The method found to be linear with calibration equation [y = 0.79x + 0.054] and a regression coefficient (r2) value of 0.996. The limits of detection and quantification for the enantiomers were 2.3 μg/spot and 6.7 μg/spot, respectively. The recovery of the enantiomers isolated from TLC plates was in the range of 76–85%.



中文翻译:

左氧氟沙星为手性选择剂的索他洛尔对映体拆分薄层色谱方法的开发

在这项工作中,使用市售的,含有羧基的手性纯药物,即左氧氟沙星被用作手性选择剂,用于拆分索他洛尔。通过在硅胶浆料中混合左氧氟沙星制备TLC板。索他洛尔的外消旋混合物在22(±2)°C下以MeCN-MeOH-H 2 O(5.2:2.0:0.8,V / V; pH = 5.0)作为流动相应用在TLC板上。根据手性选择剂的浓度,pH和温度优化了分离条件,以成功分离。观察到分辨率值为2.6。从TLC板分离如此分离的对映异构体,并使用各种技术表征。发现该方法与校准方程为线性[ y = 0.79 x  + 0.054],回归系数(r 2)值为0.996。对映体的检出限和定量限分别为2.3μg/点和6.7μg/点。从薄层色谱板分离出的对映体的回收率在76%至85%之间。

更新日期:2021-01-07
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