Zhang Tong, Nguyen Dung, Franco Pilar
Chiral Technologies Europe, Parc d'innovation, Bd Gonthier d'Andernach, Illkirch Cedex, France.
J Sep Sci. 2006 Jul;29(10):1517-24. doi: 10.1002/jssc.200600128.
Routinely used in our laboratories at analytical scale, an evaporative light scattering detector (ELSD) has proved to be versatile in the detection of enantiomeric resolution using chiral stationary phases by HPLC. Though this kind of detector has been widely used in various domains, its application in enantiomeric resolution has not been discussed in the literature and is found to have very specific features especially in the quantitative perspective. In contrast with the UV detection, the peak area from ELSD for both enantiomers of a racemic mixture may not be the same. This complicates the assessment of the enantiomeric purity of unknown samples. This current work deals with some practical aspects in the detection of enantiomers and in accurate quantitative determination of enantiomeric purity by ELSD. Effects of analyte nature (more precisely molecular weight and volatility), peak shape and peak shape difference between enantiomers on the quantitative integration by ELSD are discussed in connection with the UV-detection results. The calibration for quantitative enantiomeric analysis and its effectiveness are demonstrated.
蒸发光散射检测器(ELSD)在我们实验室的分析规模中经常使用,已证明它在通过高效液相色谱法(HPLC)使用手性固定相检测对映体拆分方面用途广泛。尽管这种检测器已在各个领域广泛使用,但其在对映体拆分中的应用在文献中尚未被讨论,并且发现它具有非常特殊的特性,特别是从定量角度来看。与紫外检测相反,外消旋混合物的两种对映体通过ELSD得到的峰面积可能不相同。这使得未知样品对映体纯度的评估变得复杂。这项当前工作涉及对映体检测以及通过ELSD准确定量对映体纯度的一些实际方面。结合紫外检测结果,讨论了分析物性质(更确切地说是分子量和挥发性)、峰形以及对映体之间的峰形差异对ELSD定量积分的影响。展示了对映体定量分析的校准及其有效性。