溶胶-凝胶法制备四种环糊精衍生物毛细管气相色谱柱  

Preparation of Stationary Phases of Four β-Cyclodextrin Derivatives for Gas Chromatography by Sol-Gel Technique

作　　者：葛晓霞[1] 齐美玲[2] 李良[2] 华菲[1] 邵青龙[2] 傅若农[2] 

机构地区：[1]中国人民武装警察部队学院,河北廊坊065000 [2]北京理工大学理学院化学系,北京10008

出　　处：《色谱》2005年第3期305-307,共3页Chinese Journal of Chromatography

摘　　要：采用溶胶凝胶法制备了七(2,3,6-三O乙基)-β-环糊精(全乙基-β-CD)、七(2,3,6-三-O-丙基)-β-环糊精(全丙基-βCD)、七(2,3,6-三-O-辛基)β环糊精(全辛基βCD)和2,6-二-O-苄基βCD4种环糊精衍生物毛细管气相色谱柱。在制备方法上,仿照一般动态法,大大简化了制备过程,缩短了制备时间。所得色谱柱的理论塔板数在3000/m左右,能够很好地分离苯衍生物的位置异构体,尤其对难分离的二甲苯、甲酚等取得了理想效果(α>1),其中溶胶凝胶法制备的全烷基(乙基、丙基、辛基)化环糊精衍生物柱的分离能力优于2,6位苄基衍生化的环糊精柱。同一根柱不同次进样和不同柱之间表现出良好的重复性,保留时间的相对标准偏差小于8.5%;对使用大约40次后的溶胶凝胶柱重新进行测试,柱效下降不明显,说明该类色谱柱的稳定性良好。Heptakis(2,3,6-tri-O-ethyl)-β-cyclodextrin (CD) (perethylated-β-CD), heptakis(2,3,6-tri-O-propyl)-β-CD (perpropylated-β-CD), heptakis(2,3,6-tri-O-octyl)-β-CD (peroctylated-β-CD), and (2,6-di-O-benzyl)-β-CD were used as stationary phases to prepare columns for gas chromatography by sol-gel technique. The method of coating the columns is similar to the dynamic method and the time required was shortened. Chromatographic characteristics such as column efficiency (around 3000 plates/m), column stability and reproducibility (relative standard deviation below 8.5%) were studied. The columns exhibited good separation ability for disubstituted benzene isomers, especially for xylenes and cresols. In addition, the three peralkylated-β-CD columns offer better selectivity than the (2,6-di-O-benzyl)-β-CD column.

关 键 词：溶胶-凝胶技术 全烷基-β-环糊精 2 6-二-O-苄基-β-环糊精 毛细管气相色谱柱 

分 类 号：O658[理学—分析化学]