Ilisz István, Fodor Gábor, Iványi Róbert, Szente Lajos, Tóth Géza, Péter Antal
Department of Inorganic and Analytical Chemistry, University of Szeged, H-6720 Szeged, Dóm tér 7, Hungary.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Nov 1;875(1):273-9. doi: 10.1016/j.jchromb.2008.05.020.
Direct capillary zone electrophoretic methods were developed for the separation of the enantiomers of unnatural beta-methyl-amino acids such as erythro- and threo-beta-methylphenylalanine, beta-methyltyrosine, beta-methyltryptophan and beta-methyl-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid. Capillary zone electrophoresis was carried out using sulfopropylated-alpha-CD (SP2-alpha-CD), sulfopropylated-beta-CD (SP2-beta-CD) both with a degree of substitution of 2 moles/mole cyclodextrin, and sulfopropylated-beta-CD (SP4-beta-CD) with a degree of substitution of 4moles/mole beta-cyclodextrin. The effects of selector and buffer concentrations, electrolyte pH and applied voltage were studied on the separation efficiency. Varying the electrophoretic conditions with application of 20 kV, hydrodynamic injection, unmodified silica capillary, three different buffers (borate, phosphate and acetate) and modified cyclodextrins as chiral selectors all compounds investigated are nearly baseline resolved. The elution sequence was determined in most cases.
已开发出直接毛细管区带电泳方法,用于分离非天然β-甲基氨基酸的对映体,如赤藓糖型和苏阿糖型β-甲基苯丙氨酸、β-甲基酪氨酸、β-甲基色氨酸和β-甲基-1,2,3,4-四氢异喹啉-3-羧酸。使用取代度为2摩尔/摩尔环糊精的磺丙基化-α-环糊精(SP2-α-CD)、磺丙基化-β-环糊精(SP2-β-CD)以及取代度为4摩尔/摩尔β-环糊精的磺丙基化-β-环糊精(SP4-β-CD)进行毛细管区带电泳。研究了选择剂和缓冲液浓度、电解质pH值和施加电压对分离效率的影响。通过施加20 kV电压、采用流体动力学进样、未改性硅胶毛细管、三种不同缓冲液(硼酸盐、磷酸盐和醋酸盐)以及改性环糊精作为手性选择剂来改变电泳条件,所有研究的化合物几乎都能实现基线分离。在大多数情况下确定了洗脱顺序。