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有机氟键合相高效液体色谱填料的研究——Ⅳ.1,1,2,2-四氢-7-三氟甲基十二氟辛基键合相填料
STUDIES ON ORGANIC FLUORO-BONDED PHASE AS HPLC PACKING Ⅳ. 1, 1, 2, 2-Tetrahydro-7-trifluoromethyldodecafluorooxtyl Bonded Phase Packing
【摘要】 <正> 在研究了以全氟辛酰胺丙基三乙氧基硅烷与硅胶反应制得的键合相高效液体色谱用填料(FN-YWG)的基础上,我们又制备了以1,1,2,2-四氢-7-三氟甲基十二氟辛基三氯硅烷作为改性剂与硅胶反应的另一种含氟的氟烃键合相填料,控制其有机层的键合量制备了既可用于正相又可用于反相色谱的填料. 实验一、试剂和仪器 1,1,2,2-四氢-7-三氟甲基十二氟辛基三氯硅烷,(CF3)2CF(CF2)4(CH2)2SiCl3,参考文献方法制备,为无色透明液体,沸点79~80℃/7mm;F113为精馏品,沸点46.5~47.6℃,经5A分子筛处理;YWG,5μ和10μ粒度,青岛硅胶;YWG-C18H37,10μ粒度,
【Abstract】 A fluoroalkylbonded phase useed as HPLC packing has been prepared from silica (5μ) and 1, 1, 2, 2-tetrahydro-7-trifluoromethyldodecafluorooctyltrichlorosilane, (CF3)2CF(CF2)4CH2CH2SiCl3. By controlling the surface concentration of the organic ligand, we prepared the packing which may be used either in normal phase or in reverse phase mode. Comparing with the perfluoroamide bonded phase packing previously prepared by us, it not only has the same chromatographic performance to give a much shorter retention time for polar steroidal compounds, to improve the peak symmetry and reduce tailing, but also more hydrophobic and less polar in nature. This fluoroalkyl bonded phase packing gives a good separation in nonaqueous reverse phase mode towards some cholenic acids which formerly can only be separated by ion exchange or reverse phase chromatography and show severe tailing on silia gel column. On the other hand, the separation of phenols and polyhydroxy steroids are also successful on this column in reverse phase mode.
- 【文献出处】 化学学报 ,Acta Chimica Sinica , 编辑部邮箱 ,1982年12期
- 【被引频次】1
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