D-吡喃葡萄糖基异硫氰酸酯柱前衍生化高效液相色谱法分离胺类对映异构体  被引量:3

Separation of Amine Enantiomer by High Performance Liquid Chromatography with D-Glycosyl-isothiocyanate as Pre-column Derivatizing Reagent

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作  者:邓小娟[1] 周维义[1] 李文斌[1] 

机构地区:[1]天津大学分析中心,天津300072

出  处:《分析测试学报》2007年第3期381-384,共4页Journal of Instrumental Analysis

摘  要:以2,3,4,6-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)为手性衍生化试剂,对8种氨基酸和2种手性药物进行手性拆分研究。考察了衍生化时间和试剂用量、流动相组成、流动相pH值对分离的影响。结果表明,样品在合适的色谱条件下,能快速达到基线分离。该法用于测定1,2-二胺基环己烷的对映异构体过量(ee)值,得到了满意的结果,方法简易、快速。对某些不对称合成中的胺类化合物的ee值测定及日常生活中氨基酸异构体的分析具有一定的应用价值。The separation of eight amino acids and some β-adrenergic blockers were investigated using 2,3,4,6-tetra-O-acetyl-(β-D-glycosyl )-isothiocyanate (GITC) as the pre-column derivatizing reagent and reversed phase high performance liquid chromatography with methanol - 1% triethylamine/acetic as mobile phase. The effects of the derivatizing time, the amount of GITC, the composition and pH of the mobile phase on the enantioseparation were discussed. The method has been applied to the determination of the excess(ee) value of 1,2-diaminocyclohexane with satisfactory results. The proposed method is feasible, rapid and reliable.

关 键 词:吡喃葡萄糖基异硫氰酸酯 DL-氨基酸 高效液相色谱 对映体拆分 

分 类 号:O657.72[理学—分析化学] Q517[理学—化学]

 

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