Irish Separation Science Cluster, National Centre for Sensor Research, Dublin City University, Glasnevin, Dublin 9, Ireland.
J Chromatogr A. 2010 Apr 2;1217(14):2138-46. doi: 10.1016/j.chroma.2010.02.007. Epub 2010 Feb 10.
A new method for the fixation of polymethacrylate monoliths within titanium tubing of up to 0.8 mm I.D. for use as a chromatographic column under elevated temperatures and pressures is described. The preparation of butyl methacrylate-ethylene dimethacrylate-based monolithic stationary phases with desired porous structures was achieved within titanium tubing with pre-oxidised internal walls. The oxidised titanium surface was subsequently silanised with 3-trimethoxysilylpropyl methacrylate resulting in tight bonding of butyl methacrylate porous monolith to the internal walls, providing stationary phase stability at column temperatures up to 110 degrees C and at operating column pressure drops of >28 MPa. The titanium housed monoliths exhibited a uniform and dense porous structure, which provided peak efficiencies of up to 59,000 theoretical plates per meter when evaluated for the separation of small molecules in reversed-phase mode, under optimal conditions (achieved at 15 microL/min and temperature of 110 degrees C for naphthalene with a retention factor, k=0.58). The developed column was applied to the reversed-phase isocratic separation of a text mixture of pesticides.
一种将高达 0.8 毫米内径的钛管内的聚甲基丙烯酸甲酯整体固定，以在高温高压下用作色谱柱的新方法被描述。在具有预氧化内壁的钛管内制备了具有所需多孔结构的丁基甲基丙烯酸酯-二乙烯基苯基整体固定相。随后，用 3-三甲氧基硅丙基甲基丙烯酸酯对氧化钛表面进行硅烷化处理，导致丁基甲基丙烯酸酯多孔整体固定相与内壁紧密结合，在高达 110°C 的柱温下和在 28MPa 以上的操作柱压降下提供固定相稳定性。钛外壳整体式固定相具有均匀且致密的多孔结构，在反相模式下对小分子进行分离时，在最佳条件下（在 15μL/min 和 110°C 的温度下，萘的保留因子 k=0.58），其理论塔板数高达 59000 块/米。所开发的色谱柱用于反相等度分离农药混合物。
