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A Silica Monolithic Column with Chemically Bonded l-Pipecolic Acid as Chiral Stationary Phase for Enantiomeric Separation of Dansyl Amino Acids by CEC-MS

机译:以化学键合的L-哌柯酸为手性固定相的硅胶整体柱,用于通过CEC-MS分离丹磺酰基氨基酸的对映体

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摘要

A silica monolithic column chemically modified with l-pipecolic acid as chiral stationary phase has been developed for chiral separation of dansyl amino acids by capillary electrochromatography-mass spectrometry (CEC-MS). The monolithic column was prepared by a sol-gel process and subsequent chemical modification by l -pipecolic acid as chiral selector with 3-glycidoxypropyltrimethoxysilane as spacer. Interestingly, it was found that the l -pipecolic acid-modified monolithic column can hold copper(II) ions tightly after loading Cu(II) ions during column preparation and conditioning and allows CEC separation to be conducted based on chiral ligand exchange with MS detection by a mobile phase without copper ions. It has been demonstrated that the chiral monolithic column operates well for enantioseparation of several dansyl amino acids by CEC-MS.
机译:已经开发了用1-哌啶酸作为手性固定相进行化学修饰的硅胶整体柱,用于通过毛细管电色谱-质谱(CEC-MS)手性分离丹磺酰基氨基酸。整体柱通过溶胶-凝胶法制备,随后通过1-哌啶酸作为手性选择剂,以3-环氧丙氧基丙基三甲氧基硅烷作为间隔物进行化学修饰。有趣的是,发现L-哌酸改性的整体柱可在色谱柱制备和调节过程中加载Cu(II)离子后紧紧固定铜(II)离子,并允许基于手性配体交换和MS检测进行CEC分离通过没有铜离子的流动相已经证明手性整体柱通过CEC-MS对几种丹磺酰基氨基酸的对映体分离操作良好。

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