Han Haifeng, Li Jing, Wang Xusheng, Liu Xia, Jiang Shengxiang
Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, P. R. China; Graduate University of Chinese Academy of Sciences, Chinese Academy of Sciences, Beijing, P. R. China.
J Sep Sci. 2011 Aug;34(16-17):2323-8. doi: 10.1002/jssc.201100050. Epub 2011 May 19.
An ionic liquid (IL) was introduced into the organic-silica hybrid monolithic column as the stationary phase for capillary electrochromatography (CEC). The monolithic silica matrix containing chloropropyl functional group was prepared by the in situ co-condensation of tetramethoxysilane and (3-chloropropyl)-trimethoxysilane via a sol-gel process and chemical modification with N-methylimidazole. The electroosmotic flow of the IL-modified hybrid monolithic column was reversed at acidic pH and the morphology of the column was characterized by scanning electron microscope. Four aromatic hydrocarbons were completely separated with 40% acetonitrile phosphate buffer as the mobile phase and seven inorganic ions were efficiently separated with the phosphate buffer on the column in CEC. Reproducibilities of migration time for four aromatic hydrocarbons (benzene, naphthalene, anthracene, chrysene) were acceptable on IL-modified hybrid monolithic columns. Relative standard deviations of run-to-run (n=5), peak area-to-peak area (n=5), day-to-day (n=3) and column-to-column (n=3) were in the range of 0.72-0.88, 1.47-5.40, 2.44-4.99 and 3.01-8.11%, respectively.
将离子液体(IL)引入有机-二氧化硅杂化整体柱中作为毛细管电色谱(CEC)的固定相。通过溶胶-凝胶法,由四甲氧基硅烷和(3-氯丙基)-三甲氧基硅烷原位共缩合,制备含有氯丙基官能团的整体二氧化硅基质,并使用N-甲基咪唑进行化学改性。IL改性杂化整体柱的电渗流在酸性pH下发生反转,并用扫描电子显微镜对柱的形态进行了表征。以40%乙腈磷酸盐缓冲液为流动相,在CEC中,四种芳烃完全分离;以磷酸盐缓冲液为流动相,在该柱上七种无机离子被有效分离。在IL改性杂化整体柱上,四种芳烃(苯、萘、蒽、芘)迁移时间的重现性良好。批内(n = 5)、峰面积-峰面积(n = 5)、日间(n = 3)和柱间(n = 3)的相对标准偏差分别在0.72 - 0.88%、1.47 - 5.40%、2.44 - 4.99%和3.01 - 8.11%范围内。