原子转移自由基聚合法制备新型亲水作用色谱固定相及其性能评价

Preparation of Hydrophilic Interaction Chromatographic Stationary Phase Using Surface-Initiated Atom Transfer Radical Polymerization and Its Chromatographic Properties

以自制的6.0μm单分散大孔交联聚氯甲基苯乙烯-二乙烯基苯(Poly(4-vinylbenzylchloride-co-divi-nylbenzene),PCMS/DVB)微球为基质和引发剂,CuCl和自行合成的三[(2-二甲基氨基)乙基]胺(Tris[2-(dimeth-ylamino)ethyl]amine,Me6TREN)组成混合催化体系,使4-乙烯基吡啶(4-Vinyl pyridine,4-VP)在甲苯中进行原子转移自由基聚合,制得4-乙烯基吡啶聚合物,单体4-乙烯基吡啶的接枝率为8.55%。将该聚合物与正溴丁烷反应制得新型亲水色谱固定相。在亲水作用色谱模式下,流速1 mL/min,乙腈-水为流动相可分离5种芳胺化合物和4种酚类化合物。在离子交换色谱模式下,6 mmol/L Na2CO3-5.5 mmol/L NaHCO3为淋洗液可分别分离5种无机阴离子和4种短链有机酸。结果表明,此固定相对极性化合物和无机阴离子具有良好的分离性能,是一种性能优异的亲水作用色谱固定相。

Atom transfer radical polymerization（ATRP） of poly-4-vinylpyridine-grafted PCMS/DVB beads were synthesized by using 6.0 μm monodisperse macroporous poly（4-vinylbenzylchloride-co-divinylbenzene）（PCMS/DVB） beads as initiator,CuCl and tris[2-（dimethylamino）ethyl] amine（Me6TREN） as catalyst and ligand in toluene.A new kind of hydrophilic interaction chromatographic（HILIC） stationary phase was synthesized by chemical modified of the poly-4-vinylpyridine-grafted PCMS/DVB beads.The grafting rate of poly-4-vinylpyridine was 8.55%.The column was tried as chroma-tographic packing for the separation of amines and hydroxybenzenes by HILIC modes and inorganic anions and organic acids by IC modes.The results showed that five amines and four hydroxybenzenes were completely separated in 10 min by acetonitrile-water as mobile phase with isocratic elution using the synthesized hydrophilic interaction chromatographic stationary phase.By using 6 mmol/L Na2CO3-5.5 mmol/L NaHCO3 as eluent,five inorganic anions and four organic acids had good linear relationship and low detection limit by IC model.The effect of water content in mobile phase on the retention of amines was evaluated.The stationary phase has good chromatographic properties for separation of polar compounds and inorganic anions.