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Fast preparation of polystyrene-based monolith using microwave irradiation for micro-column separation

机译:微波辐射快速制备聚苯乙烯基整体柱用于微柱分离

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The conventional analytical HPLC was successfully developed for micro-column separation by using a simple eluate splitting system, a self-preparation of monolithic column and an on-capillary column detector in our laboratory. A typical polystyrene-based monolith was quickly prepared inside the fused-silica capillary, which in situ polymerization was carried out in 10 min by microwave irradiation. The reactant solution consisted of styrene (ST) as a functional monomer, divinylbenzene (DVB) as a cross-linking agent, toluene and isooctane as porogenic solvents, and azobisisobutyronitrile (AIBN) as an initiator. The monolith was proved to form in the center of the capillary and adhered to the column inner wall by the scanning electron micrograph. Its chromatographic behaviors were evaluated in detail by varying the flow rate and percentage of mobile phases, and under the optimal condition, baseline separation of the model analytes including thiourea, benzene, toluene, ethylbenzene was obtained with a highest theoretical plate number near 11,290 N/m by the developed capillary HPLC. Furthermore, the stability and porosity of the prepared monolith were systematically investigated by a simple flow method.
机译:通过使用简单的洗脱液分离系统,一体式色谱柱的自我制备和毛细管柱内检测器,成功地开发了用于微柱分离的常规分析型HPLC。在熔融石英毛细管内部快速制备了典型的聚苯乙烯基整体材料,并通过微波辐照在10分钟内进行原位聚合。反应物溶液由作为功能单体的苯乙烯(ST),作为交联剂的二乙烯基苯(DVB),作为致孔剂的甲苯和异辛烷以及作为引发剂的偶氮二异丁腈(AIBN)组成。通过扫描电子显微照片证明了整体结构在毛细管的中心形成并粘附在色谱柱内壁上。通过改变流速和流动相的百分比来详细评估其色谱行为,并在最佳条件下,获得了模型分析物(包括硫脲,苯,甲苯,乙苯)的基线分离,理论塔板数最高,接近11,290 N /通过开发的毛细管HPLC进行分析。此外,通过简单的流动方法系统地研究了所制备整料的稳定性和孔隙率。

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