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以微晶纤维素、3,5-二甲基苯基异氰酸酯和3-(三乙氧基硅)丙基异氰酸酯为原料,通过区域选择法合成了6位带有三乙氧基硅基团的纤维素-二(3,5-二甲基苯基氨基甲酸酯)衍生物,利用三乙氧基硅基团的分子间缩聚将纤维素衍生物高效的固定到硅胶基质上,制备了交联型纤维素手性固定相。在正己烷-异丙醇(体积比4:1),流速1 mL/min,检测波长230 nm时,甲霜灵对映体得到了很好的分离,分离度(Rs)为4.36。此外,还探讨了流动相的配比,不同醇类改性剂对拆分效果的影响,优化了色谱条件。结果表明,交联型纤维素手性固定相对甲霜灵对映体具有较好的手性拆分能力,并且允许使用含有氯仿和四氢呋喃的流动相。
Using microcrystalline cellulose, 3,5-dimethylphenyl isocyanate and 3- (triethoxysilyl) propyl isocyanate as starting materials, 6-position fibers with triethoxysilane groups were synthesized by regioselective method Bis (3,5-dimethylphenylcarbamate) derivative, the cellulose derivative is efficiently immobilized on the silica gel matrix by intermolecular polycondensation of triethoxysilane groups to prepare a crosslinked Cellulose chiral stationary phase. The enantiomers of metalaxyl were well separated with n-hexane-isopropanol (4: 1), flow rate of 1 mL / min and detection wavelength of 230 nm. The resolution was 4.36. In addition, the ratio of mobile phase, the effect of different alcohol modifiers on resolution and the optimization of chromatographic conditions were also discussed. The results show that the crosslinked cellulose chiral stationary phase has good chiral resolution ability to metalaxyl enantiomers and allows the use of a mobile phase containing chloroform and tetrahydrofuran.