Normandie Univ., UR, EA 3233, Sciences et Méthodes Séparatives, FR 3038, I.R.C.O.F., Rue Tesnière, F-76821 Mont Saint Aignan Cedex, France; Laboratoire de Chimie Organique, Université Libre de Bruxelles (U.L.B.), Avenue F. D. Roosevelt 50, CP160/06, 1050 Brussels, Belgium.
J Chromatogr A. 2013 Nov 29;1318:207-16. doi: 10.1016/j.chroma.2013.10.007. Epub 2013 Oct 10.
New polyethylene-glycol-based sol-gels containing cyclodextrin or calix[6]arene derivatives have been synthesized. An original method for sol-gel preparation and capillary column coating, which consumes smaller quantities of selectors and allows for control of their amounts in the stationary phase, is reported herein. The new stationary phases exhibited excellent column efficiencies over a large range of temperatures and thermal stability up to 280°C. The cyclodextrin derivative generally showed the best separation factors for aromatic positional isomers. The calix[6]arene derivative exhibited the best selectivity for the polychlorobiphenyl congeners and some polycyclic aromatic hydrocarbon isomers. The relationship between the structure and the chromatographic properties of the selectors is discussed. The tert-butyl groups on the upper rim of the calix[6]arene were found to possibly play an important role in the recognition of solutes. The incorporation of the cyclodextrin derivative into the sol-gel matrix did not affect its enantioselective recognition capabilities.
已合成了含有环糊精或杯[6]芳烃衍生物的新型聚乙二醇基溶胶-凝胶。本文报道了一种新的溶胶-凝胶制备和毛细管柱涂层方法,该方法消耗的选择剂较少,并可控制固定相中的选择剂用量。新的固定相在很宽的温度范围内表现出优异的柱效和高达 280°C 的热稳定性。环糊精衍生物通常对芳族位置异构体表现出最佳的分离因子。杯[6]芳烃衍生物对多氯联苯同系物和一些多环芳烃异构体表现出最佳的选择性。讨论了选择剂的结构与色谱性能之间的关系。杯[6]芳烃上边缘的叔丁基可能在溶质识别中起重要作用。将环糊精衍生物掺入溶胶-凝胶基质中不会影响其对映选择性识别能力。