摘要
建立柱前衍生－液相色谱－荧光检测法同时测定水中草甘膦和氨甲基膦酸的方法。水样经芴甲氧羰酰氯衍生化后取上清液进样，采用 ODS C 18柱，以水（5 mmol ／L 乙酸铵）－乙腈作为流动相进行梯度洗脱，采用荧光检测器进行检测。实验通过加入柠檬酸三钠，解决了实际水样中金属阳离子的干扰问题。草甘膦和氨甲基膦酸在一定范围内线性良好（r ＝0．9973～0．9990），回收率为92．2％～102％，相对标准偏差为4．3％～8．5％，方法检出限为1．29μg ／L 和1．84μg ／L。
A method for simultaneous determination of glyphosate and aminomethylphosphonic acid residues in water was developed by pre-column derivatization followed with high performance liquid chromatography （HPLC）-fluorescence detection.9-Fluorenylm-ethyl chloroformate was selected as the derivatization reagent.After derivatization and extraction,the upper aqueous phase was ana-lyzed.HPLC was achieved on an ODS C18 column by linear gradient elution using 5 mmol ammonium acetate-acetonitrile as the mo-bile phase,and fluorescence detector was used for detection.By adding trisodium citrate,the interference from metal cations was ef-fectively eliminated.The results showed that good linear relationships （r =0.997 3 ~0.999 0）were exhibited in the range 10.0 ~500 μg /L for both compounds.The recoveries ranged from 92.2% to 102%,with the relative standard deviations of 4.3% ~8.5%.The detection limits were 1 .29 μg /L and 1 .84 μg /L for glyphosate and aminomethylphosphonic acid,respectively.This method was simple,rapid,sensitive and accurate.It was suitable for simultaneous determination of glyphosate and aminometh-ylphosphonic acid in surface water.
出处
《环境监控与预警》
2015年第2期13-16,19,共5页
Environmental Monitoring and Forewarning
基金
江苏省环境监测科研基金资助项目(1301)
