Singh Manisha, Malik Poonam, Bhushan Ravi
Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667, India.
Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667, India
J Chromatogr Sci. 2016 May-Jun;54(5):842-6. doi: 10.1093/chromsci/bmw014. Epub 2016 Feb 18.
A new chromatographic method has been developed for direct enantioresolution of (RS)-baclofen by ligand-exchange thin-layer chromatography (TLC) adopting two different approaches; (A) TLC plates were prepared by mixing the ligand exchange reagents (LER) with silica gel slurry and the chromatograms were developed with different achiral solvents or solvents having no chiral additive, and (B) the LER consisting of Cu(II)-L-amino acid complex was used as chiral mobile phase additive and the plain plates of silica gel having no chiral selector were used. Cu(II) acetate and four L-amino acids (namely, L-tryptophan, L-histidine, L-proline and L-phenylalanine) were used for the preparation of LERs. Spots were located by the use of iodine vapor. Effect of temperature and the mole ratio of Cu(II)-to-amino acid on enantioresolution were also studied. The results for the two methods have been compared, and the issue of involvement of the Cu(II) cation for the best performance of the two methods has been discussed with respect to the same mobile phase. L-Trp proved to be a good ligand using a common mobile phase in each case.
已开发出一种新的色谱方法,通过配体交换薄层色谱(TLC)采用两种不同方法直接拆分(RS)-巴氯芬的对映体;(A)通过将配体交换试剂(LER)与硅胶浆料混合制备TLC板,并用不同的非手性溶剂或无手性添加剂的溶剂展开色谱图,以及(B)将由Cu(II)-L-氨基酸络合物组成的LER用作手性流动相添加剂,并使用无手性选择剂的普通硅胶板。醋酸铜和四种L-氨基酸(即L-色氨酸、L-组氨酸、L-脯氨酸和L-苯丙氨酸)用于制备LER。斑点通过碘蒸气定位。还研究了温度和Cu(II)与氨基酸的摩尔比对对映体拆分的影响。比较了两种方法的结果,并针对相同流动相讨论了Cu(II)阳离子对两种方法最佳性能的影响问题。在每种情况下,使用常见流动相时,L-Trp被证明是一种良好的配体。