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On-line two-dimensional LC: a rapid and efficient method for the determination of enantiomeric excess in reaction
Qi Liu1, Xinyu Jiang, Haixing Zheng
1School of Chemistry and Chemical Engineering, Central South University, Changsha, P.R. China.
Abstract:
A novel LC-based method for the determination of enantiomeric excess (ee) in a sample mixture has been developed by employing on-line 2D LC. The orthogonal separation system is composed of an NH2 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 1D HPLC were all <1.03%) have been obtained. Compared with the traditional method for the determination of ee, on-line 2D HPLC can be used in real time and holds great potential in the time-saving determination of ee in asymmetric synthesis.
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