提出了柱前衍生-固相萃取-高效液相色谱法测定饮用水中草甘膦和氨甲基膦酸。水样经9-芴基甲基三氯甲烷衍生和C18固相萃取小柱净化后,洗脱液采用Waters Atlantis T3色谱柱分离,流动相为甲醇-0.02 mol·L-1乙酸铵溶液(60+40),荧光检测器激发波长为266 nm,发射波长为315 nm。草甘膦和氨甲基膦酸的质量浓度在5.00~500 μg·L-1范围内与其峰面积呈线性关系,检出限均为0.002 μg·L-1。对水样进行加标回收试验,草甘膦和氨甲基膦酸的回收率分别在84.4%~92.0%和87.8%~96.8%之间,相对标准偏差(n=6)分别在1.2%~4.3%和1.1%~4.0%之间。该方法适用于水厂出水水样中草甘膦和氨甲基膦酸的同时测定。

A method of SPE-HPLC coupled with pre-column derivatization was proposed for the determination of glyphosate and aminomethylphosphonic acid in drinking water. Water sample was derived with FMOC-Cl and purified by C18 solid phase extraction column. The derivatives were separated on an Atlantis T3 column with a mixture of methanol and 0.02 mol·L-1 of ammonium acetate (60+40) as mobile phase. The wavelengths of fluorescence excitation and emission used were 266 nm and 315 nm respectively. The linear relationship between the peak area and the mass concentration of glyphosate and aminomethylphosphonic acid were in the range of 5.00-500 μg·L-1, with detection limits (3S/N) of 0.002 μg·L-1. The recovery rates measured by adding standard samples to water sample were in the range of 84.4%-92.0% and 87.8%-96.8% for glyphosate and aminomethylphosphonic acid respectively, with RSD (n=5) in the range of 1.2%-4.3% and 1.1%-4.0% respectively. The method was used for simultaneous determination of glyphosate and aminomethylphosphonic acid in water samples of water supply plants.