文献类型：期刊文献

中文题名：析因设计法优化制备聚(DVB)型整体柱及分离小分子物质的应用

英文题名：OPTIMAL PREPARATION OF POLY(DIVINYLBENZENE) MONOLITHIC COLUMN WITH FACTORIAL DESIGN FOR SEPARATION OF SMALL MOLECULES

作者：杨朔[1];徐环昕[2];刘坐镇[2];邬行彦[1]

机构：[1]华东理工大学生物反应器国家重点实验室,上海200237;[2]上海华震科技有限公司,上海200237

年份：2009

卷号：25

期号：1

起止页码：70

中文期刊名：离子交换与吸附

外文期刊名：Ion Exchange and Adsorption

收录：CSTPCD;;Scopus;北大核心:【北大核心2008】；CSCD:【CSCD2011_2012】；

语种：中文

中文关键词：析因设计;整体柱;高效液相色谱;半高峰宽分离度(R1/2)

外文关键词：Factorial design; Monolithic column; Hioh performance liquid chromatography （HPLC）; Resolution of peak width at half height （R1/2）.

摘要：以二乙烯基苯(DVB)为单体,十二烷醇和甲苯为制孔剂,在引发剂偶氮二异丁腈(AIBN)的作用下,直接以Φ4.6×50mm色谱柱为模具,通过原位聚合制备了聚(二乙烯基苯)型整体柱。通过析因设计,以十二烷醇占反应混合物体积比,二乙烯基苯占反应混合物体积比,偶氮二异丁腈所占聚合物质量比3因素,以整体柱对小分子的分离度为响应指标进行了3因素2水平全析因实验。结果表明,引发剂的量对分离度的影响最大,其次为十二烷醇占反应混合物体积比与引发剂占聚合物质量比的交互作用和3因素交互作用,而其他效应,如十二烷醇占反应混合物体积比,DVB占反应混合物体积比,十二烷醇与DVB的交互作用,DVB与引发剂的交互作用的影响较小,可以忽略;从而得到了分离小分子物质的最优配方;通过测定整体柱的比表面积,孔径和孔容分布对其进行表征。所制备的整体柱,能够通过高效液相色谱系统对苯,乙苯和萘这3种小分子物质进行分离。分离条件为:100×4.6mmI.D.色谱柱,流动相为乙腈:水=80:20(v/v),流速1mL/min,检测峰值254nm。色谱柱背压5MPa,分离时间10min。
A monolithic column of macroporous poly （divinylbenzene） has been prepared by free radical polymerization within the confines of a Ф50×4.6mm I.D. chromatographic stainless steel tube. For reaching the best separation and low back pressure, a 23 factorial design was used with dodecanol proportion, DVB proportion and AIBN dosage as the three main variables. The result shows that the AIBN dosage was the most effective variable, and the next effective were the interaction effect of dodecanol proportion and AIBN dosage, and interaction effect of the three main variables. The others, such as DVB proportion, dodecanol proportion, and their interaction effect exerted negligible effects. The characteristic feature of the column was studied, including specific surface area, pore volume and distribution, and pore diameter as well. Using this monolithic, benzene ethylbenzene and naphthalene can be well separated on a HPLC system. The separation conditions were： column 100×4.6mm I. D. with mobile phase of acetonitrilewater （80：20 v/v）, flow-rate was hnL/min and UV detection at 254nm. Back pressure of column was 5MPa, separation time was 10min.