高效液相色谱β-环糊精键合固定相直接拆分硫代和硒代缩水甘油醚对映异构体  

Chiral Separation of Thioglycidyl Ether and Glycidylselenide on Cyclodextrin Bonded Stationary Phase via High Performance Liquid Chromatography

作　　者：于兆文[1] 周志强[1] 蒋生祥[1] 陈立仁[1] 

机构地区：[1]中国科学院兰州化学物理研究所,兰州730000

出　　处：《色谱》1999年第4期363-365,共3页Chinese Journal of Chromatography

基　　金：中国科学院重点项目基金

摘　　要：用两种不同的方法合成了β-环糊精键合固定相。通过对硝基苯胺异物体的拆分，对键合相进行了评价。拆分了3种硫代缩水甘油醚和2种未见文献报道的硒代缩水甘油醚。β- Cyclodextrin bonded chiral stationary phases (CD-CSP) were prepared after the method of Armstrong (CD-CSP Ⅰ ) and of Huang Tianbao (CD-CSP Ⅱ ). With the separation of o-,m-p- nitroaniline,it was found that the chromatographic properties of CD-CSP Ⅱ was superior to that of CD-CSP Ⅰ. Three racemes of thioglycidyl ethers and two racemes of glycidylselenides were resolved on CD-CSP Ⅱ via high performance liquid chromatography. The mobile phase consisted of different volume ratios of methanol/0. 3%triethylammonium acetate buffer solution(pH 5), and the eluate was detected with a UV-visible detector at a wavelength of 254 um. With the increase of methanol volume ratio in the mobile phase, the retention time decreased rapidly, but within the range of methanol valume ratio 40/100 to 50/100, the separation factor only decreased slightly. The racemes examined contained aromatic groups and hydroxy groups which can form inclusion complexes and hydrogen bonding interactions with β-cyclodextrin. The chiral separation of the racemes is successful with the mobile phase of V(methanol): V(buffer)= 40: 60.

关 键 词：硫代缩水甘油醚 硒代缩水甘油醚 拆分 对映体 

分 类 号：O657.720.3[理学—分析化学] O627.61[理学—化学]