Tailored ring-opening metathesis polymerization derived monolithic media prepared from cyclooctene-based monomers and cross-linkers
Tailored ring-opening metathesis polymerization derived monolithic media prepared from cyclooctene-based monomers and cross-linkers
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DOI：
10.1021/ma0609883
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发表时间：
2006-08-08
期刊：
影响因子：
5.5
通讯作者：
Buchmeiser, Michael R.
中科院分区：
文献类型：
--
作者：
Bandari, Rajendar;Prager-Duschke, Andrea;Buchmeiser, Michael R.
以顺式环辛烯（COE）为单体，三（环辛-4-烯-1-基氧基）甲基硅烷（CL）为交联剂，甲苯为致孔剂，异丙醇为大孔剂，合成了开环易位聚合（ROMP）整体式介质。以RuCl 2（Py）（2）（1，3-Mes（2）-咪唑啉-2-亚基）（CHC 6 H5）（Mes = 2，4，5-三甲基苯基，Py =吡啶）和吡啶为调节剂制备了具有不同组成的整体载体，并通过反相尺寸排阻色谱（ISEC）和电子显微镜进行了表征。将尺寸为3 × 100 mm的整料用于分离五种蛋白质的混合物，即，核糖核酸酶A、溶菌酶、胰岛素、细胞色素c和肌红蛋白。这些化合物的半制备性分离，在不到150秒内通过应用梯度洗脱实现。峰半宽（Ω（0.5））< 6 s，分辨率（R-s）始终> 1.2。新型载体的官能化原位完成，并通过在整体结构上接枝不同量的7-氧杂降冰片-5-烯-2，3-二羧酸酐来举例说明。通过这种方法，实现了高达86 μ mol/g的羧酸负载，相当于0.71wt%。
The synthesis of ring-opening metathesis polymerization ( ROMP) derived monolithic media prepared from cis-cyclooctene (COE) as monomer, tris(cyclooct-4-ene-1-yloxy) methylsilane ( CL) as cross-linker, toluene as microporogen, and 2-propanol as macroporogen is described. Monolithic supports with varying composition in terms of COE, CL, microporogen, and macroporogen were prepared using RuCl2(Py)(2)(1,3-Mes(2)-imidazolin-2-ylidene)(CHC6H5) (Mes = 2,4,5-trimethylphenyl,Py =pyridine) and pyridine as modulator and characterized via inverse size exclusion chromatography (ISEC) and electron microscopy. Monoliths 3 x 100 mm in size were used for the separation of a mixture of five proteins, i.e., ribonuclease A, lysozyme, insulin, cytochrome c, and myoglobin. Semipreparative separation of these compounds was achieved within less than 150 s by applying gradient elution. Peak half-widths (omega(0.5)) were < 6 s, and resolution (R-s) was > 1.2 throughout. Functionalization of the novel support was accomplished in situ and exemplified by grafting various amounts of 7- oxanorborn-5-ene- 2,3-dicarboxylic anhydride on the monolithic structure. By this approach, carboxylic acid loadings up to 86 mu mol/g, corresponding to 0.71 wt %, were realized.