Rapid Determination of Nine Polar Pesticide Residues in Water by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry
A method based on direct injection-ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established for the rapid determination of glyphosate,aminomethylphosphonic acid,n-acetyl glyphosate,n-methyl glyphosate,glufosinate,n-acetamidomethyl phosphate,3-methylphosphinico propionic acid,n-acetyl glufosinate and ethephon residues in a environmental water.The water samples were filtered through a 0.22 μm filter membrane or a PLS solid phase extraction column combined with a 0.22 μm filter membrane to remove impurities,then the filtrate was directly subjected to quantitative analysis without derivatization.The analytes were separated on a Dikma Polyamino HILIC column(150 mm×2.0 mm,5 μm),and gradient elution was carried out using a pH=11 ammonium formate-ammonia buffer solution and acetonitrile as the mobile phase.The data were collected by negative electrospray ionization in the multiple reaction monitoring(MRM)mode.The results showed that the correlation coefficients(r)of the linear calibration curves were greater than 0.999 in the corresponding linear ranges(0.20-50.0 μg/L).The detection limits of the analytes were 0.04-0.08 μg/L.The quantitation limits were 0.12-0.24 μg/L.The recoveries of the nine targets were in the ranges 88.9％-105％at low,medium,and high spiked levels,respectively.The corresponding relative standard deviations were in the ranges 2.8％-8.2％.This method is advantageous over the traditional derivatization method because of its simple operation,good reproducibility,and high accuracy.Furthermore,the matrix interference effect is absent.Thus,this method is suitable for analyzing glyphosate,aminomethylphosphonic acid,n-acetyl glyphosate,n-methyl glyphosate,glufosinate,n-acetamidomethyl phosphate,3-methylphosphinico propionic acid,n-acetyl glufosinate and ethephon residues in environmental water samples.
Ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)GlyphosateGlufosinate and their metaboliteWater
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