以聚乙二醇/甲醇为二元致孔剂的新型磺酸甜菜碱型两性离子亲水毛细管整体柱的合成与色谱评价

使用新型二元致孔剂聚乙二醇(PEG)/甲醇,以N,N-二甲基-N-甲基丙烯酰胺基丙基-N,N-二甲基-N-丙烷磺酸内盐(SPP)为单体,季戊四醇三丙烯酸酯(PETA)为交联剂,偶氮二异丁腈(AIBN)为引发剂,通过原位聚合法制备磺酸甜菜碱型两性离子亲水毛细管整体柱。对各反应物的配比进行了优化。结果表明,当单体与致孔剂的质量比为1∶2.5,并且致孔剂中PEG与甲醇的质量比为1∶2,单体内部SPP与PETA的质量比为1∶1,AIBN为总质量的0.1%时为最优配比;PEG/甲醇二元致孔剂的加入实现了对整体柱内部孔径大小的调节,得到了结构更为均一,渗透性、机械稳定性良好的毛细管整体柱,并且理论塔板数与传统制备方法相比有显著提高,在毛细管液相色谱模式下最高可达2.4×105塔板/m。将制备的整体柱应用于毛细管液相色谱和加压毛细管电色谱分离酚类、核苷类等极性小分子混合物,得到了很好的分离效果。

Synthesis and chromatographic evaluation of sulfobetaine-based capillary zwitterionic hydrophilic monolithic column using a binary porogenic agent of polyethylene glycol/methanol

Sulfobetaine-based capillary zwitterionic hydrophilic monolithic columns were synthesized with a novel binary porogenic agent of polyethylene glycol (PEG)/methanol. The polymer was prepared with (3-(metharyloylamino) propyl) dimethyl (3-sulfopropyl) ammonium hydroxide inner salt (SPP) as monomer, pentaerythritol triacrylate (PETA) as crosslinker, and azobisisobutyronitrile (AIBN) as initiator. In order to optimize the properties, the contents of the polymerization mixture were investigated. The optimum preparation conditions were as follows: the mass ratio of monomer and porogenator=1:2.5; the mass ratio of SPP and PETA=1:1 in the monomer; the mass ratio of PEG and methanol=2:1 in the binary porogenic agent; the content of the initiator (AIBN) =0.1% (m/m). With the binary porogenic agent of PEG/methanol addition, good mechanical stability, homogeneous column bed, good permeability and narrow pore size distribution were obtained. In the capillary liquid chromatography mode, the hydrophilic monolith provided column efficiency up to 2.4×10⁵ plates/m which was much higher than that fabricated by traditional method without PEG/methanol. The columns were used in capillary liquid chromatography and pressurized capillary electrochromatography for the separation of a mixture of phenols, nucleosides and so on.