化学学报 ›› 1982, Vol. 40 ›› Issue (1): 49-56. 上一篇    下一篇

论文

有机氟键合相高效液体色谱填料的研究 Ⅱ.全氟酰胺键合YWG的制备、性能及应用

李文华, 王锦华, 林志平   

  1. 中国科学院上海有机化学研究所
  • 投稿日期:1980-03-10 发布日期:2013-06-03
  • 通讯作者: 李文华

STUDIES ON THE FLUORO-ORGANIC BONDED Ⅱ. PREPARATION, PROPERTIES AND APPLICATION OF PERFLUOROAMIDE BONDED YWG SILICA

LI WEN-HUA, WANG JIN-HUA, LIN ZHI-PING   

  1. Shanghai Institute of Organic Chemistry, Academia Sinica
  • Received:1980-03-10 Published:2013-06-03

我们将各种不同浓度的全氟辛酰胺丙基三乙氧基硅烷溶液,分别与YWG(无定形硅胶,粒度5μ)反应,制备了各种不同有机层覆盖量的全氟酰胺键合YWG,其键合基为全氟辛酰胺丙基一乙氧基硅烷,有机层的表面浓度分别为0.24,0.61,0.88,1.26μmol/m2.这些高效液体色谱填料随着所键合有机氟基团量的增加,其极性逐渐减弱,对一些甾族极性样品所给予的保留时间愈来愈短,对滞留时间愈长的样品所产生的影响愈明显.由于此种填料在硅原子上键合了氟链,增加了憎水性,可改进极性甾族化合物峰形的对称性及拖尾因子,此填料对一些在YWG柱上不能分离的胆甾烯样品有较好的分离作用,也能用于多羟基的甾族样品的分离.

Some perfluoro-amide bonded YWG with different amount of organic coverage (3.48%,9.3%,12.67%,18.19%) have been prepared from YWG silica, with various amount of perfluorooaprylamido-propyl-triethogy-silane in CF2ClCFCl2 solution, perfluorooaprylamido-propyl-monoethogyl was proved to be the group bonded onto the surface, its surface concentrations on these packings are 0.24, 0.71, 0.88, 1.26 μM/m2 respectively. YWG silica contains the higher concentration of the fluorinated group will show the weaker polarity. These fluorinated YWG silica samples give rise to a much shorter retention time for polar steroid compounds. This effect is more obvious in the case of compounds with a longer retention time. As the flouoro-amide group is hydrophobic in nature, so it not only modifies the peak symmotry and tailing factor, but also shows good selectivety towards some compounds of oholestene series, which could not be separated on YWG silica column under normal conditions.