异喹啉酸衍生物配体交换色谱手性固定相的制备及应用  

Preparation and Application of Isoquinolinecarboxylic Acid Derivative as Chiral Stationary Phase for Ligand Exchange Chromatography

作　　者：孟庆华[1] 王圣庆[1] 郭瑛[1] 马言顺[1] 龙远德[1] 黄天宝[1] 

机构地区：[1]中国科学院成都有机化学研究所

出　　处：《分析化学》2006年第3期311-315,共5页Chinese Journal of Analytical Chemistry

摘　　要：合成了2-（2-羟基十六烷基）-（S）-1,2,3,4-四氢-3-异喹啉羧酸手性选择子,并采用动态涂渍方法,制备了一种涂渍于ODS柱上的新型手性配体交换色谱固定相.采用醋酸铜水溶液为流动相,在柱温25℃和UV254nm检测条件下,拆分了16种D,L-氨基酸对映体,其对映体选择性α和分离度Rs分别在1.09～1.67和1.0～4.8之间,并观察到D-异构体在先,L-异构体在后的色谱流出顺序.讨论了柱温、流动相的流速、pH值、Cu^2＋浓度和NH＋4对D,L-氨基酸对映体拆分的影响.A novel chiral stationary phase （C16-（S）-THIQCA） for ligand exchange high performance liquid chromatography was prepared by synthesizing 2- （ 2-hydroxyl ） hexadecyl- （ S ） -1,2,3,4-tetrahydro-3 -isoquinolinecarboxylic acid as chiral selector and coating it on octadecyl bonded silica （ODS） bonded stationary phase. The enantiomeric resolutions of 16 D,L-amino acids were achieved on C16-（S）-THIQCA by using cupric acelate aqueous solution as mobile phase, column temperature 25℃ and detection at ultraviolet 254 nm. The enantioselectivities a of the D,L-amino acids separated were found to be in the range of 1. 09 to 1. 67 with the resolution Rs ranging from 1. 0 to 4.8. The elution order of D-isomer before L-isomer was observed for all D, L-amino acids used. The effects of chromatographic conditions including flow rate, column temperature, pH, the concentration of Cu^2 ＋ and NH4^＋ on the resolutions of D, L-amino acid enantiomers were studied and discussed.

关 键 词：异喹啉酸衍生物 配体交换色谱 手性固定相 D L-氨基酸 

分 类 号：O657.75[理学—分析化学]