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使用负载颗粒整体柱通过配体交换进行对映体拆分:毛细管液相色谱与毛细管电色谱法

Enantioseparation by ligand-exchange using particle-loaded monoliths: capillary-LC versus capillary electrochromatography.

作者信息

Schmid Martin G, Koidl Julia, Wank Pamela, Kargl Gabriele, Zöhrer Helga, Gübitz Gerald

机构信息

Institute of Pharmaceutical Sciences, Department of Pharmaceutical Chemistry, Karl-Franzens-University, Universitätsplatz 1, A-8010 Graz, Austria.

出版信息

J Biochem Biophys Methods. 2007 Feb 23;70(1):77-85. doi: 10.1016/j.jbbm.2006.06.004. Epub 2006 Aug 7.

Abstract

Particle-loaded monoliths containing a polymethacrylamide backbone were prepared by suspending a silica-based chiral phase in the mixture of the monomers followed by in-situ polymerization in the capillary. As chiral selector l-4-hydroxyproline chemically bonded to 3 microm silica particles was used following the separation principle of ligand-exchange. Electrolytes containing Cu(II) ions were used. Amino acid enantiomers were separated by capillary-LC and CEC, whereby the latter showed the better resolution properties. For the chiral separation of alpha-hydroxy acids the EOF was reversed by copolymerizing diallyldimethylammonium chloride instead of vinylsulfonic acid as charge providing agent. Short columns of 6 cm were found to be sufficient in the case of CEC for baseline separations of amino acids with alpha values up to 5.

摘要

通过将基于二氧化硅的手性相悬浮在单体混合物中,然后在毛细管中进行原位聚合,制备了含有聚甲基丙烯酰胺主链的负载颗粒整体柱。按照配体交换的分离原理,使用化学键合到3微米二氧化硅颗粒上的手性选择剂L-4-羟基脯氨酸。使用含有铜(II)离子的电解质。通过毛细管液相色谱和毛细管电色谱分离氨基酸对映体,其中后者表现出更好的分离性能。对于α-羟基酸的手性分离,通过共聚二烯丙基二甲基氯化铵而不是作为电荷提供剂的乙烯基磺酸来使电渗流反转。发现在毛细管电色谱的情况下,6厘米的短柱足以对α值高达5的氨基酸进行基线分离。

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