尼索朗对映体的高效毛细管电泳电导拆分

Enantioseparation of Hexythiazox by Capillary Electrophoresis with Conductive Detection

使用自行设计的毛细管电泳柱端电导检测系统,以未涂层融硅石英毛细管(75μm×45 cm)为分离柱,用非水介质对尼索朗对映体进行了拆分。研究了缓冲溶液浓度和酸碱度、非水介质、手性拆分剂(β-CD)等因素对分离的影响。以V(甲醇):V(甲酰胺)=8:2溶液为非水介质,5 mmol/L NaAc+2 mmol/L HAc为缓冲溶液,分离电压为15 kV,在8．0～160 mg/L范围内,峰高与浓度呈良好的线性关系,线性同归方程:y= 9．4+36．8x,线性相关系数R=0．996 3,检出限为1．6 mg/L。

A method for the enantioseparation of Hexythiazox via capillary electrophoresis with conductive detection was developed. The enantiomers of Hexythiazox were baseline separated within 10 min under the following separation conditions： uncoated fused silica capillary （45 cm × 75 μm, i. d. ）, 5 mmol/L NaAc ＋ 2 mmol/L HAc ＋ 5 mmol/L β-CD （ pH = 4. 0 ） ＋ V（methanol） ： V（ N, N-Dimethylformamide ） = 8： 2 as running buffer, 15 kV separation voltage. The effect of running buffer, pH, the concentration of chiral selector, separation voltage and inject time were discussed in detail. A linearity was found between peak height （y） and mass concentration of Hexythiazox（x） in a range of 8.0 - 160 mg/L with a regression equation of y = 9.4 ＋ 36. 8x, and the correlation coefficient was 0. 996 3, and the determination limit was 1.6 mg/L.