柱前衍生高效液相色谱法测定地下水中草甘膦

Determination of Glyphosate in Groundwater by High Performance Liquid Chromatography Combined with Pre-column Derivatization

建立柱前衍生高效液相色谱法来测定地下水中草甘膦。水样经9-芴甲基氯甲酸酯衍生后,采用C18颗粒分散固相萃取净化,经PAH C18色谱柱分离,流动相为乙腈-0.2%磷酸水溶液,荧光检测器激发波长为254 nm,发射波长为315 nm。草甘膦的质量浓度在0.40~100μg/L范围内与其衍生化物对应的荧光响应峰面积线性关系良好(r=0.9998),检出限为0.089μg/L。对水样添加0.50~100μg/L进行加标回收试验,草甘膦的回收率在86.0%~98.7%,相对标准偏差(n=6)在0.28%~6.18%。方法经优化后绿色、高效,能够满足大批量地下水体中草甘膦快速检测的需求。

The determination of glyphosate in groundwater by high performance liquid chromatography(HPLC)combined with pre-columnderivatization was proposed.Water sample was derived with 9-fluorenylmethyl chloroformate(FMOC-Cl).After derivatization and extraction using C18 dispersive solid phase extraction,the upper aqueous phase was analyzed.HPLC was achieved on a PAH C18 column by gradient elution using 0.2%phosphoric acid-acetronitrile as the mobile phase,and fluorescence detector was used for detection The wavelengths of fluorescence excitation and emission used were 254 nm and 315 nm,respectively.The linear relationship between the peak area and the mass concentration of glyphosate was in the range of 0.40~100μg/L,with the detection limits of 0.089μg/L.The recovery rates measured by adding standard samples to water sample were in the range of 86.0%~98.7%,with the relative standard deviations in the range of 0.28%~6.18%(n=6).This method was green and efficient after optimization.It was suitable for the rapid determination of glyphosate in groundwater.