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在前人工作的基础上,以微晶纤维素和3,5 二甲基苯基异氰酸酯为原料合成了纤维素 三(3,5 二甲基苯基氨基甲酸酯),并将其涂敷于小粒径的氨丙基化硅胶(APS)上,制备出纤维素 三(3,5 二甲基苯基氨基甲酸酯)涂敷型硅基手性固定相。通过元素分析、红外光谱对该固定相进行了表征。用正相高效液相色谱法在该固定相上首次直接拆分了触杀型苗后除草剂氯氟草醚乙酯对映体。考察了流动相组成对对映体保留和拆分的影响,结果发现,随着异丙醇体积分数的减小,对映体的分离度逐渐增大,在异丙醇的体积分数为1 0%时,分离度已达3 95。
Based on the previous work, cellulose tris (3,5-dimethylphenyl carbamate) was synthesized from microcrystalline cellulose and 3,5-dimethylphenyl isocyanate, and coated On a small particle size aminopropylated silica gel (APS), a tris (3,5-dimethylphenylcarbamate) -coated silicon-based chiral stationary phase was prepared. The stationary phase was characterized by elemental analysis and infrared spectroscopy. For the first time, the enantiomer of the clomazone herbicide, clomazone, has been directly resolved on this stationary phase by normal-phase high performance liquid chromatography. The influence of mobile phase composition on the retention and resolution of enantiomers was investigated. The results showed that the resolution of enantiomers increased with the decrease of isopropanol volume fraction. When the isopropanol volume fraction was 10 %, The resolution has reached 3 95.