硅基寡聚砜型新型HPLC固定相的制备及其色谱性能评价

Preparation and chromatographic evaluation of a novel silica-based oligopolyethylsulfone HPLC stationary phase

以硅小球为基质,γ-氨丙基三乙氧基硅烷,环硫乙烷和过氧乙酸为改性剂,制备了硅基寡聚砜型新型液相色谱固定相。在活化的硅小球表面引入氨基,制得氨基键合相,然后氨基键合相与环硫乙烷进行开环聚合反应,在氨基键合相表面引入巯基和硫醚基,最后用过氧乙酸将其分别氧化为磺酸基和砜基,制得磺酸乙基聚乙砜基胺丙基固定相。采用元素分析进行表征,通过S和N的摩尔比确定固定相表面胺基,砜基和磺酸基的比例。在不同条件下,分别选用碱性化合物、中等极性和弱极性化合物等13种溶质对该固定相的色谱性能进行评价,证明该固定相兼有疏水作用,亲水作用和静电作用。用于实际样品测定,该固定相呈现出良好的分离选择性和较广的应用范围。

A novel silica-based oligopolyethylsulfone HPLC stationary phase functionalized with three modifiers of3-aminopropyltriethoxysilane,ethylene sulfide and peracetic acid was prepared.Silica gel reacted with 3-aminopropyltriethoxysilane to prepare the amino-bonded stationary phase(ASP).Then,mercaptoethyl-polyethyl sulfide-aminopropyl-bonded stationary phase(MPAS)was prepared by bonding sulfhydryl group and thioether group to the surface of ASP via a polymerization with ethylene sulfide.The MPAS was oxidized by peracetic acid to prepare ethyl sulfonate-polyethyl sulfone-aminopropyl-bonded stationary phase(EPAS).The stationary phase was characterized by elemental analysis.The ratios of amino,sulfone and sulfonic group on the surface of the stationary phase was determined by the molar ratio of S and N.The chromatographic properties of the EPAS were investigated by 13 kinds of solutes,such as basic compounds,medium polar compounds and weak polar compounds,under different conditions,and it was proved that the EPAS had hydrophobic,hydrophilic and electrostatic effects.The stationary phase showed good separation abilities and wide applicability in real samples detection.