高效液相色谱法拆分苯霜灵对映体

以高效液相色谱手性固定相法在对映体水平上建立了苯霜灵的分析方法。采用OD手性色谱柱,正己烷/异丙醇流动相,流速为1.0 mL/m in,检测波长206 nm,以圆二色检测器对两对映体进行出峰顺序确证并考察了其圆二色特性。结果显示,苯霜灵单一对映体在0.52~259.2 mg/L浓度范围内具有较好的线性,线性相关系数均大于0.9994,最低检出限为0.26 mg/L,在240 nm处的出峰顺序为( )/(-)。同时建立了苯霜灵对映体在土壤、水、葡萄中的残留分析方法。土壤和葡萄样品分别用丙酮和乙腈提取,水样用固相萃取法(SPE)富集净化。土壤中两对映体在0.025~2.5 mg/kg范围内的回收率为93.67%~108.95%之间;水样品在0.005~0.5 mg/L浓度范围的回收率在85.13%~100.79%之间,葡萄样品在0.04~1 mg/kg浓度范围的回收率在83.22%~106.62%之间;相对标准偏差RSD均小于6%。

Enantiomeric Analysis of Benalaxyl by High Performance Liquid Chromatography

A method for the analysis of benalaxyl enantiomers was established by high performance liquid chromatography using OD chiral stationary phase.Hexane/isopropanol mobile phase was used with a flow rate of 1.0 mL/min and detection wavelength of 206 nm.The enantiomers were identified by circular dichroism(detector).Good linearities were obtained for the two enantiomers at the concentration of 0.52-259.2 mg/L with the linear relative coefficient more than 0.9994.Limit of detection was 0.26 mg/L for both enantiomers.The residual analysis method for benalaxyl eanatiomers in soil,water and grape was also set up.Soil and grape samples were extracted by acetone and acetonitrile respectively,and water samples were extracted by C_(18) solid phase extraction(SPE).The recoveries for the two enantiomers in soil were 93.7%-109.0% at the concentration of 0.025-2.5 mg/kg,85.1%-100.8% in water at the concentration of 0.005-0.5 mg/L and 83.2%-106.6% in grape at the concentration of 0.04-1 mg/kg.The relative standard deviations were less than 6.0%.