Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (12): 1260-1264.DOI: 10.3724/SP.J.1123.2012.07031

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Determination of glufosinate residue in tea by liquid chromatography-tandem mass spectrometry coupled with precolumn derivatization

LIN Yonghui*, LIU Zhengcai, YANG Fang, QIU Yuanjin, LIU Suzhen, SU Zhijiao, ZHANG Qiong, XUE Zhimin, FANG Yu   

  1. Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China
  • Received:2012-07-17 Revised:2012-09-25 Online:2012-12-28 Published:2012-12-19

Abstract: A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for the determination of glufosinate (GLUF) residue in tea. The GLUF was extracted with water for 30 min under ultrasonication, and cleaned-up using a C18 solid phase extraction cartridge, then derived using fluorenylmethylchloroformate (FMOC-Cl) in borate buffer for 2 h. The separation was performed on a Kinetex C18 column with the mobile phases of acetonitrile and 5 mmol/L ammonium acetate aqueous solution (containing 0.2% (v/v) formic acid) in a gradient elution mode. The identification and quantification of the GLUF were carried out by MS/MS in negative electrospray ionization (ESI~) and multiple reaction monitoring (MRM) mode, the quantification analysis was performed by external standard method. The calibration curve showed good linearity in the range of 2.5~50.0 μg/L with the correlation coefficient r2>0.999. The limit of quantification (LOQ) was 0.10 mg/kg. The average recoveries of GLUF spiked at 0.10, 0.50 and 1.00 mg/kg levels in tea were between 61.6% and 81.4%, and the relative standard deviations (RSDs) were between 3.2% and 8.4%. The method is simple, rapid, sensitive, accurate and suitable for the confirmation and quantification of GLUF in tea.

Key words: glufosinate, liquid chromatography-tandem mass spectrometry (LC-MS/MS), tea, precolumn derivatization