【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 C18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=0.997 3~0.999 0),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。更多还原

【Abstract】 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-Fluorenylmethyl chloroformate was selected as the derivatization reagent. After derivatization and extraction,the upper aqueous phase was analyzed. HPLC was achieved on an ODS C18 column by linear gradient elution using 5 mmol ammonium acetate-acetonitrile as the mobile phase,and fluorescence detector was used for detection. By adding trisodium citrate,the interference from metal cations was effectively 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 aminomethylphosphonic acid in surface water.更多还原