Organic monolithic capillary columns coated with cellulose tris(3,5-dimethylphenyl carbamate) for enantioseparations by capillary HPLC
Organic monolithic capillary columns coated with cellulose tris(3,5-dimethylphenyl carbamate) for enantioseparations by capillary HPLC
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DOI：
10.1016/j.microc.2019.104011
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发表时间：
2019-09-01
影响因子：
4.8
通讯作者：
Reta, Mario
中科院分区：
文献类型：
--
作者：
Echevarria, Romina N.;Keunchkarian, Sonia;Reta, Mario
通过将手性选择剂纤维素三(3,5-二甲基苯基氨基甲酸酯)涂覆在有机聚合物上，成功制备了一种用于毛细管液相色谱中对映体分离的新型手性整体柱。这种具有优化多孔特性的聚合物是在二元致孔混合物（1-十二醇和环己醇）存在下，通过甲基丙烯酸 2-羟乙酯和二甲基丙烯酸乙二醇酯的热聚合，在预处理的熔融石英毛细管中原位制备的。将手性选择剂沉积到整体载体上以获得稳定且可重现的手性固定相。该柱在正相模式下使用，正己烷和2-丙醇的组成不同。研究了酸性或碱性添加剂对对映体拆分的影响。九种手性酸性、中性和碱性化合物（洛芬、β-阻滞剂、农药等）在短时间内得到部分或完全解析。获得的对映选择性值高达 7.1，对映分辨率高达 2.4。整体手性柱表现出良好的稳定性，保留因子的日内和日间重现性值的 RSD% 分别低至 1.5% 和 4.3%。此外，由于 RSD% 低至 12.7%，因此色谱柱制造十分稳健。这是第一篇将手性选择剂纤维素三(3,5-二甲基苯基氨基甲酸酯)成功涂覆到毛细管柱中制备的有机聚合物整料上，用于毛细管液相色谱对映体分离的报道。
A new chiral monolithic column for enantiomer separation in capillary LC was successfully prepared by coating the chiral selector cellulose tris(3,5-dimethylphenyl carbamate) onto an organic polymer. This polymer, with optimized porous properties, has been prepared in situ in pretreated fused-silica capillaries by thermal polymerization of 2-hydroxyethyl methacrylate and ethylene glycol dimethacrylate in the presence of a binary porogenic mixture (1-dodecanol and cyclohexanol). The chiral selector was deposited onto the monolithic support to obtain a stable and reproducible chiral stationary phase. The column was used under normal phase mode with different compositions of n-hexane and 2-propanol. The effect of acidic or basic additives on the enantioresolution was studied. Nine chiral acid, neutral, and basic compounds (profens, beta-blockers, pesticides, among others) were partially or completely resolved in short analysis times. Enantioselectivity values up to 7.1 and enantioresolutions up to 2.4 were obtained. The monolithic chiral column exhibited good stability, with RSD % for infra- and inter-day reproducibility values of the retention factor as low as 1.5% and 4.3%, respectively. Also, column fabrication is robust since RSD% was as low as 12.7%. This is the first report in which the chiral selector cellulose tris(3,5-dimethylphenyl carbamate) was successfully coated onto an organic polymeric monolith prepared in capillary columns for enantiomeric separations by capillary LC.