核壳型磁性APTES-Fe3O4纳米涂层柱的制备及应用
An APTES-Fe3O4 magnetic nanoparticle-coated capillary and its application in enantiomeric separation
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摘要: 以羧甲基-β-环基糊精(carboxymethyl-β-cyclodextrin，CM-β-CD)作为手性选择剂，以3-氨基丙基三乙氧基硅烷-四氧化三铁(3-aminopropyltriethoxysilane-Fe3O4，APTES-Fe3O4)磁性纳米粒吸附于毛细管内壁，在外加磁场下进行手性分离。本研究通过提供外加磁场的方式，将核壳结构的APTES-Fe3O4磁性纳米粒涂布于毛细管内壁，制备了一种核壳型磁性APTES-Fe3O4纳米涂层柱。此法操作简便，且毛细管涂层重复性好，柱寿命超过80次电泳分析。经0.01 mol/L HCl、0.001 mol/L NaOH、CH3OH和CH3CN等冲洗15 min后，涂层未发生明显变化，化学稳定性强。外加磁场去除后，作为涂层的磁性纳米粒可进行回收重复利用。首次将此涂层柱应用于手性药物的毛细管电泳拆分，成功分离了氧氟沙星、普萘洛尔对映体。结果表明，相比于未涂层柱，APTES-Fe3O4磁性纳米涂层柱能提高柱效并改善分离效果。实验考察了手性选择剂浓度、缓冲溶液pH、有机相种类及比例、运行电压等电泳条件对分离的影响，优化条件下两种药物分离度分别为1.97和1.93。
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关键词:
- 核壳型磁性纳米粒 /
- 涂层毛细管柱 /
- 手性分离 /
- 毛细管电泳 /
- APTES-Fe3O4
Abstract: A coated capillary with 3-aminopropyltriethoxysilane modified magnetic nanoparticles(APTES-MNPs)as the stationary phase was constructed and applied in enantio-separation in capillary electrophoresis. The magnetic nanoparticles coating inside the capillary columns could be easily generated by applying and removing the external magnetic field. The APTES-MNPs-coated capillary showed long lifetime, superior chemical stability and good reproducibility. It endured during more than 80 replicated analyses and was tolerant to HCl(0. 01 mol/L), NaOH(0. 001 mol/L), CH3OH and CH3CN. The APTES-MNPs-coated capillary can be applied to enantioseparation of basic drugs. Compared with the uncoated capillary system, improved separation of the tested enantiomers(ofloxacin and propranolol)were obtained in the system based on APTES-MNPs-coated capillary. Several primary parameters such as chiral selector concentration, running buffer pH, organic solvent and applied voltage, were systematically optimized in order to obtain successful chiral separation. The results indicate that the application of magnetic nanoparticles is a promising way in chiral separation. -
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