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On‐line two‐dimensional LC : A rapid and efficient method for the determination of enantiomeric excess in reaction mixtures
Author(s) -
Liu Qi,
Jiang Xinyu,
Zheng Haixing,
Su Wen,
Chen Xiaoqing,
Yang Hua
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201300412
Subject(s) - chromatography , chemistry , enantiomer , elution , high performance liquid chromatography , enantiomeric excess , reproducibility , two dimensional chromatography , analytical chemistry (journal) , enantioselective synthesis , stereochemistry , organic chemistry , catalysis
A novel LC ‐based method for the determination of enantiomeric excess ( ee ) in a sample mixture has been developed by employing on‐line 2 D LC . The orthogonal separation system is composed of an NH 2 column as the first dimension to elute the target chiral compound from the crude mixture and a chiral column as the second dimension to determine the ee of the target chiral product. A series of crude mixtures from asymmetric reactions have been directly analyzed without prepurification. Good reproducibility (intra‐ and interday precisions were all under 1.33%) and good accuracy (deviations from ee values determined by 1 D HPLC were all <1.03%) have been obtained. Compared with the traditional method for the determination of ee , on‐line 2 D HPLC can be used in real time and holds great potential in the time‐saving determination of ee in asymmetric synthesis.