色谱

色谱

• 研究简报 • 上一篇    下一篇

溶胶-凝胶法制备四种环糊精衍生物毛细管气相色谱柱

葛晓霞1,2,齐美玲2,李良2,华菲1,邵青龙2,傅若农2   

  1. 1. The Chinese People′s Armed Police Force Academy, Langfang 065000, China; 2. Department of Chemistry, School of Science, Beijing Institute of Technology, Beijing 100081, China
  • 收稿日期:2004-05-08 修回日期:1900-01-01 出版日期:2005-05-30 发布日期:1988-09-25
  • 通讯作者: 葛晓霞
  • 基金资助:

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

GE Xiaoxia1,2, QI Meiling2, LI Liang2, HUA Fei1, SHAO Qinglong2, FU Ruonong2   

  1. 1. The Chinese People′s Armed Police Force Academy, Langfang 065000, China; 2. Department of Chemistry, School of Science, Beijing Institute of Technology, Beijing 100081, China
  • Received:2004-05-08 Revised:1900-01-01 Online:2005-05-30 Published:1988-09-25

PDF

615

被引次数

27

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-β-CD)、七(2,3,6-三-O-辛基)-β-环糊精(全辛基-β-CD)和2,6-二-O-苄基-β-CD 4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。

关键词: 2,6-二-O-苄基-β-环糊精, 毛细管气相色谱柱 , 全烷基-β-环糊精, 溶胶-凝胶技术

Abstract: 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 3000 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.

Key words: (2,6-di-O-benzyl)-β-cyclodextrin, peralkylated-β-cyclodextrin, capillary gas chromatographic column , sol-gel technique