Wang Peng, Liu Donghui, Jiang Shuren, Xu Yangguang, Zhou Zhiqiang
Department of Applied Chemistry, China Agricultural University, Beijing 100094, China.
J Chromatogr Sci. 2008 Oct;46(9):787-92. doi: 10.1093/chromsci/46.9.787.
The amylose-tris(3,5-dimethylphenylcarbamate) chiral stationary phase was synthesized and used to separate the enantiomers of triazole pesticides by high-performance liquid chromatography. The mobile phase was n-hexane-isopropanol applying a flow rate of 1.0 mL/min. Six triazole pesticides were enantioselectively separated. Myclobutanil, paclobutrazol, tebuconazole, and uniconazole obtained complete separation with the resolution factors of 5.73, 2.99, 1.72, and 2.07, respectively, and imazalil and diniconazole obtained partial separation with the resolution factors of 0.79 and 0.77 under the optimized conditions. The effect of the content of isopropanol as well as column temperature on the separation was investigated. A circular dichroism detector was used to identify the enantiomers and determine the elution orders. The results showed the low temperature was good for the chiral separation except for diniconazole. The thermodynamic parameters calculated based on linear Van't Hoff plots showed the chiral separations were controlled by enthalpy.
合成了直链淀粉-三(3,5-二甲基苯基氨基甲酸酯)手性固定相,并用于通过高效液相色谱法分离三唑类农药的对映体。流动相为正己烷-异丙醇,流速为1.0 mL/min。六种三唑类农药实现了对映体选择性分离。在优化条件下,腈菌唑、多效唑、戊唑醇和烯效唑实现了完全分离,分离度分别为5.73、2.99、1.72和2.07,抑霉唑和烯唑醇实现了部分分离,分离度分别为0.79和0.77。研究了异丙醇含量以及柱温对分离的影响。使用圆二色检测器鉴定对映体并确定洗脱顺序。结果表明,除烯唑醇外,低温有利于手性分离。基于线性范特霍夫图计算的热力学参数表明,手性分离受焓控制。