β-环糊精金属有机骨架材料HPLC手性柱拆分噁唑禾草灵

Separation of Fenoxaprop Enantiomers by HPLC Column ofβ-cyclodextrin Metal-organic Framework Material

合成了以β-环糊精和间羧基苯磺酰氯为有机配体、钾离子为配位离子的金属有机骨架材料(MOF)键合在高效液相色谱硅珠上,构建了高效液相色谱(HPLC)手性固定相(β-CD-MOF-P20@SiO_(2))新型材料,以此作为HPLC固定相,在反相色谱模式下,以乙酸铵-三乙胺/乙酸缓冲液和乙腈为流动相,优化流动相配比、缓冲液pH值、浓度和流速等色谱条件,获得了噁唑禾草灵两对映体最佳分离度,可达9.89。两对映体色谱峰响应信号与消旋体浓度在6.20×10^(-6)~2.99×10^(-4) mol/L范围内的线性相关性好(r=0.996 2~0.999 9),该MOF材料为噁唑禾草灵单一对映体定性、定量及制备提供了新方法。

The synthesis of a novel material for chiral stationary phase in high-performance liquid chromatography(HPLC)by bondingβ-cyclodextrin and meta-carboxybenzenesulfonyl chloride as organic ligands,with potassium ions as coordinating ions,onto silica beads(β-CD-MOF-P20@SiO_(2))was described.In reverse phase chromatography mode,using ammonium acetate triethylamine/acetic acid buffer and acetonitrile as the mobile phase,chromatographic conditions such as mobile phase ratio,buffer pH,concentration,and flow rate were optimized.Under the optimal separation conditions,the resolution reached 9.89.The linear correlation between the chromatographic peak response signals of the two enantiomer pairs and the concentration of the racemate was good in the range of 6.20×10^(-6) to 2.99×10^(-4) mol/L(r=0.9962~0.9999).A new method for the qualitative,quantitative determination and preparation of fenoxaprop-ethyl single enantiomer was developed.