Determination of Glyphosate and Aminomethyl Phosphonic Acid Residues in Green Coffee by Solid Phase Extraction-Liquid Chromatography Tandem Mass Spectrometry
In order to provide guidance for the use of glyphosate pesticides in coffee cultivation,it is necessary to establish a detection method for analyzing glyphosate and aminomethyl phosphonic acid residues in green coffee.The green coffee powder was extracted by ultrasonic with water at room temperature,lipid-soluble components in the extracts were extracted with dichloromethane,and the supernatant were purified by PCX solid phase extraction.Derivatization reaction was happened between purified solution and 9-fluorenylmethyl chloroformate.Liquid chromatograhy-tandem mass spectrometry was used for analyzing derivative products of glyphosate and aminomethyl phosphonic acid at positive ion mode,and quantified by internal standard.The results of determination of glyphosate and aminomethyl phosphonic acid residues in green coffee by solid phase extraction-liquid chromatography tandem mass spectrometry showed that a good linear relationship was observed between glyphosate and aminomethyl phosphonic acid in the range of 2～100 ng/mL,and the average recoveries ranged from 81.8%to 97.5%at the spiked levels of 0.05,0.10 and 0.20 mg/kg with the relative standard deviations of less than 9.1%,and the limits of quantification(LOQ)of glyphosate and aminomethyl phosphonic acid were 0.04 mg/kg.The method was applied to FAPAS(19377)proficiency testing with satisfactory results which Z score was-0.4.This method had good linear relations,accuracy and precision met the requirement of quantitative analysis,it was suitable for quantitative analysis of glyphosate and aminomethyl phosphonic acid residues in green coffee.
green coffeesolid phase extractionglyphosateaminomethyl phosphonic acidliquid chromatography tandem mass spectrometry
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