胶束电动毛细管色谱法测定水中的毒死蜱含量

DETERMINATION OF CHLORPYRIFOS IN WATER BY MICELLAR ELECTROKINETIC CAPILLARY CHROMATOGRAPHY

利用胶束电动毛细管色谱(MEKC)建立了测定水中毒死蜱含量的方法,研究了检测波长、运行缓冲液的种类、浓度以及pH、有机添加剂、脱氧胆酸钠(NaDCh)的浓度和分离电压等实验条件对毒死蜱测定的影响.实验结果表明,以25 mmol.L-1硼砂(pH 9.0,含20%(V/V)乙腈和50 mmol.L-1NaDCh)作为缓冲溶液,毒死蜱能在15 min内实现很好的基线分离,线性范围为15.63—500 mg·L-1,线性相关系数为0.9998,检出限(以信噪比(S/N=3)计)为0.135 mg·L-1,加标回收率为98.91%—100.9%.精密度和稳定性实验中,峰面积和迁移时间的相对标准偏差均小于3%,表明重复性良好.

A method for chlorpyrifos determination in water based on micellar electrokinetic capillary chromatography had been developed.The assay conditions including detection wavelength,pH and the concentrations of running buffer,organic additive,the concentrations of sodium deoxycholate（NaDCh）,and the separation voltage were optimized.Under the optimized conditions（25 mmol·L-1 borate buffer（pH 9,containing 20%（V/V） acetonitrile,50 mmol·L-1 NaDCh）,chlorpyrifos was separated within 15 min,with a linear range of 15.63—500 mg·L-1（r2=0.9998） and a limit of detection（S/N=3） of 0.135 mg·L-1.It had good recoveries（98.91%—100.9%） and low relative standard deviations（below 3%）.