Determination of Glyphosate and Aminomethylphosphonic Acid Residues in Tea by Dispersive Solid-phase Extraction Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry
Determination of Glyphosate and Aminomethylphosphonic Acid Residues in Tea by Dispersive Solid-phase Extraction Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2015,34(3):335-340.
Determination of Glyphosate and Aminomethylphosphonic Acid Residues in Tea by Dispersive Solid-phase Extraction Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2015,34(3):335-340.DOI:
A method for the determination of glyphosate(PMG) and aminomethylphosphonic acid(AMPA) residues in tea was developed using dispersive solid-phase extraction(dSPE) combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were ultrasonically extracted with 0.2% formic acid,and then enriched and cleaned up with Layered Double Hydroxides(Mg-Al-LDHs) absorbent.The analytes were derived with fluorenylmethylchloroformate(FMOC-Cl) in sodium carbonate solution for 2 h.The separation of the target compounds were performed on a Phenomenex Kinetex C18 column(50 mm×2.1 mm,2.6 μm) using acetonitrile-5 mmol/L ammonium acetate(containing 0.2% formic acid) as mobile phase by gradient elution.The identification and quantification of the drugs were carried out by positive electrospray ionization(ESI+) in multiple reaction monitoring(MRM) mode,the quantification analysis was performed by the isotopically labelled internal standard method.The calibration curves showed good linearities in the range of 10-1 000 ng/mL with correlation coefficients(r2) more than 0.999.The limits of detection(LOD) and the limits of quantitation(LOQ) were 0.015 mg/kg and 0.05 mg/kg,respectively.The average recoveries of PMG and AMPA in different matrices at spiked levels of 0.05,0.1 and 1.0 mg/kg were between 866% and 95.7%,with relative standard deviations(RSDs) of 5.1%- 12.2%.The developed method is simple,rapid and sensitive,and is suitable for the rapid determination of trace PMG and AMPA residues in tea.
关键词
分散固相萃取高效液相色谱-串联质谱法茶叶草甘膦氨甲基膦酸
Keywords
dispersive solid-phase extraction(dSPE)high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)teaglyphosateaminomethylphosphonic acid