关键词: 超高效液相色谱-串联质谱法, 草甘膦, 草铵膦, 残留, 茶叶

Abstract: A rapid method was developed for the determination of glyphosate (GLY) and glufosinate-ammonium (GLUF) in tea using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with NaOH solution and after pH adjustment with HCl, the extract was cleaned up with N-(n-propyl) ethyenediamine (PSA), and then was derivatized with 9-fluorenylmethyl chlorformate (FMOC-Cl) in borate buffer solution. The derivatives of GLY and GLUF were detected with positive electrospray ionization-mass spectrometry (ESI-MS/ MS) in the multiple reaction monitoring (MRM) mode. The quantification was performed by external standard method. The method showed a good linearity (r > 0.995) in the range of 0.005–0.50 μg/mL. The limit of detection (LOD) and the limit of quantization (LOQ) were 0.05 and 0.08 mg/kg for both GLY and GLUF, respectively. At spiked levels of 0.08, 0.10, 1.0, 2.0 and 4.0 mg/kg, the recoveries of GLY and GLUF were 75.6%–95.5% and 76.0%–96.6%, with relative standard deviations (RSDs) (n = 10) of 3.24%–8.38% and 3.05%–7.85%, respectively. This method proved to be simple and rapid, and its sensitivity and accuracy could meet the requirements for the simultaneous analysis of GLY and GLUF in tea.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), glyphosate, glufosinate-ammonium, residue, tea