Gatschelhofer Christina, Schmid Martin G, Schreiner Karin, Pieber Thomas R, Sinner Frank M, Gübitz Gerald
Institute of Medical Technologies and Health Management, JOANNEUM RESEARCH, Auenbruggerplatz 20/3, A-8036 Graz, Austria.
J Biochem Biophys Methods. 2006 Nov 30;69(1-2):67-77. doi: 10.1016/j.jbbm.2006.01.010. Epub 2006 Feb 17.
Novel particle-loaded monolithic capillary electrochromatography (CEC) phases for chiral separations were prepared via ring-opening metathesis polymerization (ROMP) within the confines of fused silica columns with 200 microm i.d. using norborn-2-ene (NBE), 1,4,4a,5,8,8a-hexahydro-1,4,5,8,exo,endo-dimethanonaphthalene (DMN-H6) as monomers, 2-propanol and toluene as porogens, RuCl2(PCy3)2(CHPh) as initiator and silica-based particles containing the chiral selector. By suspending silica particles bearing the chiral selector in the polymerization mixture, particle-based monoliths are easily prepared. This approach has several advantages compared to particle-based separation media: (i) the concept of particle-based monoliths is broadly applicable, as any silica-based chiral phase can be used; (ii) they are inexpensive to prepare; and (iii) the manufacturing process is very simple, no sophisticated packing procedures or the preparation of end frits are required. To show the usefulness of this concept for chiral CEC, the chiral separation performance of particle-loaded CEC monoliths bearing teicoplanin aglycone, chemically bonded to 3 microm silica gel, was investigated for a set of glycyl-dipeptides. Particle-loaded ROMP CEC monoliths showed good separation performance for glycyl-dipeptides.
通过开环易位聚合(ROMP),在内径为200微米的熔融石英柱内,以降冰片-2-烯(NBE)、1,4,4a,5,8,8a-六氢-1,4,5,8,外,内-二亚甲基萘(DMN-H6)为单体,2-丙醇和甲苯为致孔剂,RuCl2(PCy3)2(CHPh)为引发剂,并使用含有手性选择剂的二氧化硅基颗粒,制备了用于手性分离的新型颗粒负载整体毛细管电色谱(CEC)固定相。通过将带有手性选择剂的二氧化硅颗粒悬浮在聚合混合物中,可轻松制备基于颗粒的整体柱。与基于颗粒的分离介质相比,这种方法具有几个优点:(i)基于颗粒的整体柱概念具有广泛的适用性,因为任何基于二氧化硅的手性固定相都可以使用;(ii)它们制备成本低廉;(iii)制造过程非常简单,不需要复杂的填充程序或制备终端烧结片。为了证明这一概念对手性CEC的实用性,研究了负载替考拉宁苷元(化学键合到3微米硅胶上)的颗粒负载CEC整体柱对一组甘氨酰二肽的手性分离性能。颗粒负载的ROMP CEC整体柱对甘氨酰二肽显示出良好的分离性能。