Hybrid monolithic columns coated with cellulose tris(3,5-dimethylphenyl-carbamate) for enantioseparations in capillary electrochromatography and capillary liquid chromatography.
Hybrid monolithic columns coated with cellulose tris(3,5-dimethylphenyl-carbamate) for enantioseparations in capillary electrochromatography and capillary liquid chromatography.
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DOI：
10.1016/j.chroma.2012.09.022
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发表时间：
2012-12
期刊：
影响因子：
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通讯作者：
Junjie Ou;Hui Lin;Shouwan Tang;Zhenbin Zhang;Jing Dong;Hanfa Zou
中科院分区：
文献类型：
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作者：
Junjie Ou;Hui Lin;Shouwan Tang;Zhenbin Zhang;Jing Dong;Hanfa Zou
以(3-氯丙基)-三甲氧基硅烷(CPTMS)和四甲氧基硅烷(TMOS)为原料，采用溶胶-凝胶法合成了3-氯丙基-三甲氧基硅烷(CPTMS)和四甲氧基硅烷(TMOS)杂化整体毛细管柱，并在毛细管电色谱(CEC)和毛细管液相色谱(CLC)中原位涂布了纤维素三(3，5-二甲基苯基氨基甲酸酯)(CDMPC)对映体。在包覆前，用二乙烯三胺(DETA)直接修饰CP-SiO_2杂化整体柱，通过亲核取代反应引入NH_2官能团，从而为CEC生成较强的EOF。优化了包被条件，得到了稳定的手性固定相，用于手性拆分。结果表明，在毛细管电泳色谱(CEC)中，外消旋安息香在30 mg/mLCDMPC包被的混合整体柱上得到了基线分离，而在CLC中，几种外消旋体在包被60 mg/mLCDMPC的CP-SiO_2杂化整体柱上以RP和NP模式成功地分离。
A hybrid monolithic capillary column synthesized with (3-chloropropyl)-trimethoxysilane (CPTMS) and tetramethoxysilane (TMOS) via sol–gel chemistry was in situ coated with cellulose tris(3,5-dimethylphenyl-carbamate) (CDMPC) for enantioseparations in capillary electrochromatography (CEC) and capillary liquid chromatography (CLC). Prior to coating, the prepared CP-silica hybrid monolith was straightforwardly modified with diethylenetriamine (DETA) to introduce NH2functionalities via the nucleophilic substitution reaction, which generate the stronger EOF for CEC. The coating condition was optimized to obtain a stable and reproducible chiral stationary phase for enantioseparation. The results indicated that racemic benzoin was baseline separated on the resulting hybrid monolith coated with 30mg/mL CDMPC in CEC, while several racemates were successfully enantioseparated on the resulting CP-silica hybrid monolithic column coated with 60mg/mL CDMPC in CLC with RP and NP modes.