Speybrouck David, Doublet Charline, Cardinael Pascal, Fiol-Petit Catherine, Corens David
Analytical Sciences - Discovery Sciences, Janssen Research & Development, a Division of Janssen-Cilag, Campus de Maigremont, CS10615, F-27106 Val de Reuil Cedex, France.
Analytical Sciences - Discovery Sciences, Janssen Research & Development, a Division of Janssen-Cilag, Campus de Maigremont, CS10615, F-27106 Val de Reuil Cedex, France.
J Chromatogr A. 2017 Aug 11;1510:89-99. doi: 10.1016/j.chroma.2017.06.049. Epub 2017 Jun 17.
Supercritical Fluid Chromatography is frequently used to efficiently handle separations of enantiomers. The separation of basic analytes usually requires the addition of a basic additive in the mobile phase to improve the peak shape or even to elute the compounds. The effect of increasing the concentration of 2-propylamine as additive on the elution of a series of basic compounds on a Chiralpak-AD stationary phase was studied. In this study, unusual additive concentrations ranging from 0.3% to 10% of 2-propylamine 2-propylaminein the modifier were explored and the effect on retention, peak shape, selectivity and resolution was evaluated. The addition of a large quantity of additive allowed to drastically improve the selectivity and the resolution, and even enantiomers elution order reversal was observed by changing the concentration of basic additive. The role of the ratio additive/modifier appeared a key to tune the enantioselectivity. Finally, the impact of these drastic conditions on the column material was evaluated.
超临界流体色谱法常用于高效地处理对映体的分离。分离碱性分析物通常需要在流动相中添加碱性添加剂，以改善峰形，甚至洗脱化合物。研究了增加作为添加剂的2-丙胺浓度对一系列碱性化合物在Chiralpak-AD固定相上洗脱的影响。在本研究中，探索了改性剂中2-丙胺浓度范围为0.3%至10%的异常添加剂浓度，并评估了其对保留、峰形、选择性和分离度的影响。添加大量添加剂可显著提高选择性和分离度，甚至通过改变碱性添加剂的浓度观察到对映体洗脱顺序的反转。添加剂/改性剂的比例似乎是调节对映选择性的关键。最后，评估了这些剧烈条件对柱材料的影响。
