超高效液相色谱-串联质谱法同时直接测定草甘膦和草铵膦及其代谢物

Simultaneous Direct Determination of Glyphosate and Glufosinate and their Metabolites in Water by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

样品经高速冷冻离心后,采用SIELC Obelisc N色谱柱(50 mm×2.1 mm,5μm)分离,以乙腈和0.1%甲酸水溶液为流动相进行等度洗脱。质谱采用电喷雾离子源电离、以负离子扫描,多反应监测模式检测。结果表明,5种待测物在1~500μg/L质量浓度范围内线性良好,相关系数均大于0.99;回收率为82.8%~95.5%,相对标准偏差(RSD,n=6)为1.73%~4.77%。该方法快速、灵敏、准确,适合水中草甘膦、氨甲基膦酸、乙酰氨甲基膦酸、草铵膦和3-(甲基膦基)丙酸的同时分离分析。

A method has been developed for the simultaneous determination of Organophosphorus Herbicides and their metabolites in water by ultra-high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS).The sample was centrifuged by high speed freezing.The target compounds were separated on an Obelisc N column with the gradient elution of acetonitrile and water(containing 0.1%formic acid).The five components were determined in the modes of electrospray positive ionization(ESI-)and multiple reaction monitoring(MRM).The linear ranges were 1-500μg/L with the correlation coefficients higher than 0.99.The recoveries of the five compounds ranged from 82.8%to 95.5%,with the relative standard deviations(RSDs)of 1.73%-4.77%.The method showed high sensitivity and good reproducibility.It is suitable for the simultaneous detection of glyphosate,aminomethylphosphonic acid,N-acetyl-aminomethylphosphonic acid,glufosinate,3-hydroxy(methyl)phosphinoyl in water.