利用表面预烯基化纳米硅胶颗粒制备新型液相色谱整体柱
|
摘要
本文利用表面预烯基化的无机纳米硅胶颗粒作为交联剂,甲基丙烯酸(MAA)与2-二甲基乙基胺甲基丙烯酸酯(DAMA)作为有机功能单体,偶氮二异丁腈(AIBN)作为引发剂,甲醇、环己醇和水作为三元致孔剂,在内径为150μm的石英玻璃管中通过原位聚合制备了一种有机与无机杂化两性离子交换整体柱。确定了整体柱的最佳制备条件:聚合混合物为纳米硅胶颗粒(7.5 mg)+DAMA(11.25μL)+MAA(11.25μL)+环己醇(35μL)+甲醇(17.5μL)+水(17.5μL)+AIBN(0.2 mg);反应时间为10 h;反应温度为60℃。分离条件优化后,基于离子交换机理分离了一组无机阴离子,基于亲水作用和离子交换混合机理分离了一组有机胺类阳离子。
An organically-inorganically hybrid zwitterionic monolithic column was prepared for liquid chromatography by in-situ polymerization of pre-alkenated silica nanoparticles, methacrylic acid(MAA) and 2-dimethylethylamine methacrylate(DAMA) in the presence of ternary porogens consisting of 2, 2-Azobisisobutyronitrile(AIBN),cyclohexanol, methanol and water in a 150 μm i.d. fused silica capillary. The optimal preparation conditions of the column were selected. The polymerization mixture was composed of 7.5 mg of inorganic silica nanoparticles, 11.25 μL of DAMA, 11.25 μL of MAA, 35 μL of cyclohexanol, 17.5 μL of methanol, 17.5 μL of water, and 0.2 mg of AIBN; the polymerization time was 10 h; the polymerization temperature was 60℃. After separation conditions were optimized, a group of inorganic anions was separated based on ion-exchange mechanism and a group of organic cations were separated based on a mixed mechanism of ion-exchange and hydrophilic interaction.
An organically-inorganically hybrid zwitterionic monolithic column was prepared for liquid chromatography by in-situ polymerization of pre-alkenated silica nanoparticles, methacrylic acid(MAA) and 2-dimethylethylamine methacrylate(DAMA) in the presence of ternary porogens consisting of 2, 2-Azobisisobutyronitrile(AIBN),cyclohexanol, methanol and water in a 150 μm i.d. fused silica capillary. The optimal preparation conditions of the column were selected. The polymerization mixture was composed of 7.5 mg of inorganic silica nanoparticles, 11.25 μL of DAMA, 11.25 μL of MAA, 35 μL of cyclohexanol, 17.5 μL of methanol, 17.5 μL of water, and 0.2 mg of AIBN; the polymerization time was 10 h; the polymerization temperature was 60℃. After separation conditions were optimized, a group of inorganic anions was separated based on ion-exchange mechanism and a group of organic cations were separated based on a mixed mechanism of ion-exchange and hydrophilic interaction.
引文
[1]Jaafar J,Watanabe Y,Ikegami T,et al.Anion exchange silica monolith for capillary liquid chromatography[J].Anal Bioanal Chem,2008(391):2551-2556.
[2]Zhang Z B,Lin H,Qu J J,et al.Preparation of phenyl-silica hybrid monolithic column with “one-pot” process for capillary liquid chromatography[J].Journal of Chromatography A,2012(1228):263-269.
[3]Li X Y,Cristina L Q.Advances in separation science applied to metabonomics[J].Electrophoresis,2008(29):3724-3736.
[4]Gu J F,Wu W J,Huang M W,et al.Application of high-performance liquid chromatography coupled with linear ion trap quadrupole orbitrap mass spectrometry for qualitative and quantitative assessment of shejin-liyan granule supplements[J].Molecules,2018(23):884-895.
[5]Bagwe R P,Yang C,Hilliard L R,et al.Optimization of dye-doped silica nanoparticles prepared using a reverse microemulsion method[J].Langmuir,2004(19):8336-8342.
[6]李金祥,邹温然,杨芮萌,等.利用表面预烯基化纳米硅胶颗粒制备有机与无机杂化强阳离子交换液相色谱整体柱[J].德州学院学报,2018(2):29-32.
[2]Zhang Z B,Lin H,Qu J J,et al.Preparation of phenyl-silica hybrid monolithic column with “one-pot” process for capillary liquid chromatography[J].Journal of Chromatography A,2012(1228):263-269.
[3]Li X Y,Cristina L Q.Advances in separation science applied to metabonomics[J].Electrophoresis,2008(29):3724-3736.
[4]Gu J F,Wu W J,Huang M W,et al.Application of high-performance liquid chromatography coupled with linear ion trap quadrupole orbitrap mass spectrometry for qualitative and quantitative assessment of shejin-liyan granule supplements[J].Molecules,2018(23):884-895.
[5]Bagwe R P,Yang C,Hilliard L R,et al.Optimization of dye-doped silica nanoparticles prepared using a reverse microemulsion method[J].Langmuir,2004(19):8336-8342.
[6]李金祥,邹温然,杨芮萌,等.利用表面预烯基化纳米硅胶颗粒制备有机与无机杂化强阳离子交换液相色谱整体柱[J].德州学院学报,2018(2):29-32.