%0 Journal Article
%T Optimization of preparation of poly (glycidyl methacrylate- divinylbenzene) monolithic column with orthogonal experiments for separation of small molecules<br>正交试验法优化制备用于小分子物质分离的聚(甲基丙烯酸缩水甘油酯-二乙烯基苯)型整体柱
%A MA Wei
%A XU Huanxin
%A LIU Zuozhen
%A NING Fanghong
%A <br>马伟
%A 徐环昕
%A 刘坐镇
%A 宁方红
%J 色谱
%D 2010
%I 
%X A monolithic column of macro porous poly(glycidyl methacrylate-divinylbenzene) (poly(GMA-DVB)) has been prepared by free radical polymerization within the confines of a chromatographic stainless steel tube (50 mm×4.6 mm).For the best separation and low back pressure,orthogonal experiments were carried out with V(cyclohexanol)∶ V(dodecanol),V(GMA)∶ V(DVB) and BPO dosage as the three main factors.The characteristic feature of the column,including specific surface area,pore volume as well as pore diameter distribution,was studied by scanning electron microscopy (SEM),mercury intrusion porosimetry analysis and BET analysis.The obtained optimum preparation conditions were that the volume ratio of GMA,DVB,cyclohexanol and dodecanol was 0.825∶0.825∶1.32∶2.03 and the BPO dosage was 0.7%(mass percentage),then it was heated at 70 ℃ for 24 h.Using this monolithic column,benzene and ethylbenzene and a drug of oxiracetam can be well separated on a high performance liquid chromatographic (HPLC) system equipped with a ultraviolet (UV) detector at 254 nm.A solution of acetonitrile-water (50∶50,v/v) for the separation of benzene and ethylbenzene,and acetonitrile-water (80∶20,v/v) for the separation of oxiracetam were used as mobile phases at a flow rate of 1 mL/min.The theoretical plate number was 37 000 plates/m and the resolution of peak width at half height (R_(1/2)) was 7.14.The separation time was less than 10 min.The monolithic column prepared by this method is reproducible and has high column efficiency.It is an economical method to prepare monolithic column,which can be applied to separate small molecules.
%K poly(glycidyl methacrylate-divinylbenzene)
%K monolithic column
%K preparation
%K high performance liquid chromatography (HPLC)
%K small molecular<br>聚(甲基丙烯酸缩水甘油酯-二乙烯基苯)
%K 整体柱
%K 制备
%K 高效液相色谱
%K 小分子物质
%U http://www.alljournals.cn/get_abstract_url.aspx?pcid=6E709DC38FA1D09A4B578DD0906875B5B44D4D294832BB8E&cid=6579068328FE643F&jid=4D81E042D77AFEC6881D14759692069C&aid=0CA6314C3035889EDE5A7217BEE3D33B&yid=140ECF96957D60B2&vid=D3E34374A0D77D7F&iid=0B39A22176CE99FB&sid=A58CF3BAE79427D0&eid=E114CF9BB47B65BE&journal_id=1000-8713&journal_name=色谱&referenced_num=0&reference_num=15