高效液相色谱法对氯氟吡氧乙酸1-甲基庚酯对映体的拆分

Separation of Fluroxypyr-meptyl Enantiomers by High Performance Liquid Chromatography

为了对氯氟吡氧乙酸1-甲基庚酯对映体进行分离分析,合成了纤维素-三(3,5-二甲基苯基氨基甲酸酯)(CDMPC),并将其涂敷在球形氨丙基硅胶(APS)上制成液相色谱手性固定相,采用该固定相在正相色谱条件下首次成功地对氯氟吡氧乙酸对映体进行了拆分。考察了流动相中异丙醇含量以及流速对拆分的影响,并对拆分的机理进行了探讨。当流动相组成为正已烷+异丙醇(99∶1,体积比),流速为0.5mL/min时,对映体分离因子a为1.16,分辨率Rs为1.13。结果表明,氯氟吡氧乙酸1-甲基庚酯对映体在氨丙基硅胶柱上能得到较好的拆分,依此可建立一个有效的对映体分析方法。

In order to separate and analyze fluroxypyr-meptyl enantiomers, cellulose-tris(3,5-dimethyl-phenylcarbamate) (CDMPC) was prepared and coated on aminopropylated spherical gel as a chiral stationary phase(CSP). Fluroxypyr-meptyl enantiomers were firstly and directly (separated) on this CSP by normal-HPLC, the effects of 2-propanol content in mobile phase and the flow rate on separation were investigated, and the interactive mechanism between CDMPC and enantiomers was discussed. When the mobile phase composed of hexane and 2-propanol(99∶1, V/V)and the flow rate was 0.5 mL/min,the separation factor(a)and the resolution factor(R_s) was 1.16 and 1.13,respectively. The results showed that good enantioseparation was achieved on CDMPC, accordingly a validated method can be developed to analyze fluroxypyr-meptyl (enantiomers.)