水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究

张蓓蓓1; 张立志2; 章勇1

引用本文:	张蓓蓓1，张立志2，章勇1.水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究[J].环境监控与预警,2015,7(2):13-16
	ZHANG Bei bei1, ZHANG Li zhi2, ZHANG Yong1.Coupling Pre column Derivatization with High Performance Liquid Chromatography for Determination of Glyphosate and AminomethylPhosphonic Acid in Water[J].Environmental Monitoring and Forewarning,2015,7(2):13-16

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水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究
张蓓蓓1，张立志2，章勇1^1,2
1.国家环境保护地表水环境有机污染物监测分析重点实验室，江苏省环境监测中心，江苏南京 210036;2. 南京农业大学，江苏南京 210095

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1.29 μg/L和1.84 μg/L。

关键词: 草甘膦氨甲基膦酸芴甲氧羰酰氯柱前衍生柱前衍生-液相色谱法地表水

DOI：

分类号:O657.7+2

基金项目:江苏省环境监测科研基金资助项目（1301）

Coupling Pre column Derivatization with High Performance Liquid Chromatography for Determination of Glyphosate and AminomethylPhosphonic Acid in Water

ZHANG Bei bei1, ZHANG Li zhi2, ZHANG Yong1^1,2

1.State Environmental Protection Key Laboratory of Monitoring and Analysis for Organic Pollutants in Surface water, Environmental Monitoring Center of Jiangsu Province, Nanjing, Jiangsu 210036, China;2. Nanjing Agricultural University, Nanjing, Jiangsu 210095, China

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.

Key words: Glyphosate Aminomethylphosphonic acid 9 Fluorenylmethyl chloroformate Pre column derivatization Surface water