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以正己烷-1,2-二氯乙烷为流动相,添加乙腈为改性剂,在酰胺类手性液相色谱柱上实现了对烯唑醇光学异构体的直接拆分。探讨了色谱柱、温度和乙腈的含量对拆分效果的影响,优化了色谱条件。实验结果显示:单独使用KR100-5CHI-DMB色谱柱时,烯唑醇中的光学异构体仅稍微分离;而单独使用Chirex3001时,烯唑醇中的光学异构体则不分离;当KR100-5CHI-DMB与Chirex 3001串联使用时,烯唑醇中光学异构体能够得到很好的分离;在流动相中加入少量的乙腈作为极性添加剂,有助于改善异构体的分离度。当流动相为正己烷-1,2-二氯乙烷-乙腈(体积比8∶1∶1),流速1.0 mL/min,检测波长254 nm,柱温10℃时,烯唑醇中光学异构体得到很好的分离,分离度(R)为3.26。结果表明,酰胺类手性液相色谱柱能有效分离烯唑醇的光学异构体,方法简便、快速。
Using n-hexane-1,2-dichloroethane as the mobile phase and acetonitrile as the modifier, the optical resolution of diniconazole enantiomers was achieved on an amide chiral column. The effects of column, temperature and acetonitrile on the resolution were discussed, and the chromatographic conditions were optimized. The experimental results showed that the optical isomers of diniconazole were only slightly separated when KR100-5CHI-DMB was used alone, while the optical isomers of diniconazole did not separate when Chirex3001 was used alone. When KR100- When 5CHI-DMB is used in combination with Chirex 3001, optical isomers in diniconazole can be well separated. Adding a small amount of acetonitrile to the mobile phase as a polar additive helps to improve the resolution of the isomers. When the mobile phase was n-hexane-1,2-dichloroethane-acetonitrile (8:1:1), the flow rate was 1.0 mL / min, the detection wavelength was 254 nm and the column temperature was 10 ℃, The structure was well resolved with a resolution (R) of 3.26. The results showed that the amide chiral liquid chromatographic column can effectively separate the optical isomers of diniconazole, the method is simple and rapid.