A new application of stopped-flow chiral HPLC: inversion of enantiomer elution order

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• 作者：Cirilli ; R. ; Ferretti ; R. ; Gallinella ; B. ; Zanitti ; L. ; Torre ; F. La
• 关键词：Enantiomer separation ; Polymeric chiral stationary phases ; Stopped-flow chiral HPLC ; Elution order reversal ; CD detection ; Temperature effects
• 刊名：Journal of Chromatography A
• 出版年：2004
• 出版时间：December 17, 2004
• 年：2004
• 卷：1061
• 期：1
• 页码：27-34
• 全文大小：423 K

文摘

A newly developed procedure to reverse the enantiomer elution order of compounds resolved on chiral stationary phases (CSPs) for HPLC is presented. The optimized analytical protocol is based on the effect of temperature on enantioselectivity and does not involve any changing in mobile phase composition or type of CSP. In essence, the approach entails variable temperature chromatography at two temperatures. The enantiomer separation is performed at a low column temperature, with stopping the flow prior to elution of the less retained enantiomer. Then, the column temperature is changed with the peaks trapped inside the column, followed by elution with the same mobile phase in reverse direction. Under these conditions, the more pronounced loss in free energy of binding for the more strongly bound enantiomer results in an inversion of the elution order. This procedure may be applied to each enantiomer pair that is separated by chiral HPLC under an appreciable enthalpy-control.