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| Determination of Glyphosate and Aminomethylphosphonic Acid Residues in Tea by Dispersive Solid-phase Extraction Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:dispersive solid-phase extraction(dSPE) high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) tea glyphosate aminomethylphosphonic acid |
| Author | Institution |
| LIU Zheng-cai*,CAI Chun-ping,LIN Yong-hui,YANG Fang,LIU Su-zhen,XU Dun-ming,PAN Ying-fen |
1．福建出入境检验检疫局福建省检验检疫技术研究重点实验室;2.厦门出入境检验检疫局 |
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| Abstract: |
| 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. |
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