分析测试学报2012，Vol.31Issue(9)：1075-1080,6.DOI:10.3969/j.issn.1004-4957.2012.09.009
新型二元致孔剂Pluronic F127/十二胺用于辛基杂化整体柱的合成与色谱性能评价
Improvement of Chromatographic Performances of C8 Hybrid Monoliths by Using a Novel Binary Porogenic Agent of Pluronic F127/Dodecylamine
摘要
Abstract
A novel binary porogenic agent of Pluronic F127/dodecylamine was used in the fabrication of C8 hybrid monoliths by the two-step acid/base sol - gel transition. Scanning electron microscope images showed that the morphology varied from particle aggregates to co-continuous structure and the sizes of macropore and skeleton decreased when F127 was added. In the meantime, F127 was also helpful for the regulation of the mesopore of the monoliths. As a result, a more fine morphology with a higher surface area was obtained which was more beneficial for small molecules analysis. In addition , the time of sol — gel transition was prolonged about 10 min when reducing the amount of dode-cylamine, which provided enough time for filling step and improved the column-to-column reproduc-ibility. The permeability of the C8 hybrid monolithic columns was calculated to be 2. 53 ×10 -13 m2 which was still satisfactory compared to the other kinds of monolithic columns. Pressure test was passed in a wide range of flow rate of mobile phase and the van Deemter curves for benzene and toluene were acceptable. The C8 hybrid monolith of the binary porogenic agent had a plate number of 49 000/m which was much higher than that of C8 monolith fabricated by traditional method without Pluronic F127. The performance of the C8 hybrid monoliths was investigated in nanoliquid chromatogra-phy - ultraviolet/mass spectrometry ( nanoLC — UV/MS) mode. Good peak shapes were obtained in the analysis of polycyclic aromatic hydrocarbons and alkylbenzens. Seven kinds of microcystins and Nod - R were also separated by the C8 hybrid monoliths. As a conclusion, the new C8 hybrid monolithic columns were easier in preparation, more convenient in the control of morphology, higher in column efficiency, and more useful in analysis of small molecules.关键词
二元致孔剂/杂化整体柱/Pluronic F127/十二胺Key words
binary porogenic agent/ hybrid monolith/ Pluronic F127/ dodecylamine分类
化学化工引用本文复制引用
单圆鸿,石先哲,窦阿波,乔利珍,李华,许国旺..新型二元致孔剂Pluronic F127/十二胺用于辛基杂化整体柱的合成与色谱性能评价[J].分析测试学报,2012,31(9):1075-1080,6.基金项目
国家自然科学基金项目(81060086,20805045) （81060086,20805045）
国家973计划课题(2012CB720801) （2012CB720801）
