Wieder Wolfgang, Lubbad Said H, Trojer Lukas, Bisjak Clemens P, Bonn Guenther K
Institute of Analytical Chemistry and Radiochemistry, Leopold-Franzens University, Innrain 52a, 6020 Innsbruck, Austria.
J Chromatogr A. 2008 May 16;1191(1-2):253-62. doi: 10.1016/j.chroma.2007.11.070. Epub 2007 Nov 29.
Hydrophobic organo-silane based monolithic capillary columns were prepared by thermally initiated free radical polymerisation within the confines of 200 microm i.d. fused silica capillaries. A novel crosslinker, namely bis(p-vinylbenzyl)dimethylsilane (BVBDMS), was copolymerised with p-methylstyrene (MS) in the presence of 2-propanol and toluene, using alpha,alpha'-azoisobutyronitrile (AIBN) as initiator. Monolithic capillary columns, differing in the total monomer, microporogen content and microporogen nature were fabricated and the chromatographic efficiency of each monolith, regarding the separation of proteins, peptides and oligonucleotides, was evaluated and compared. Changes in monolith morphology were monitored by scanning electron microscopy (SEM). Porosity and specific surface areas of the supports were studied by means of mercury intrusion porosimetry and BET measurements, respectively. Pressure drop vs. flow rate measurements proved the prepared poly(p-methylstyrene-co-bis(p-vinylbenzyl)dimethylsilane) (MS/BVBDMS) monoliths to be mechanically stable and swelling propensity (SP) factors of 0.78-1.10 indicate high crosslinking homogeneity.
通过在200微米内径的熔融石英毛细管内进行热引发自由基聚合反应,制备了基于疏水性有机硅烷的整体式毛细管柱。使用α,α'-偶氮二异丁腈(AIBN)作为引发剂,在2-丙醇和甲苯存在下,将一种新型交联剂双(对乙烯基苄基)二甲基硅烷(BVBDMS)与对甲基苯乙烯(MS)进行共聚。制备了总单体、致孔剂含量和致孔剂性质不同的整体式毛细管柱,并对每种整体柱在蛋白质、肽和寡核苷酸分离方面的色谱效率进行了评估和比较。通过扫描电子显微镜(SEM)监测整体柱形态的变化。分别通过压汞法和BET测量研究了载体的孔隙率和比表面积。压降与流速的测量结果证明,制备的聚(对甲基苯乙烯 - 共 - 双(对乙烯基苄基)二甲基硅烷)(MS/BVBDMS)整体柱具有机械稳定性,0.78 - 1.10的溶胀倾向(SP)因子表明交联均匀性高。