色谱2012，Vol.30Issue(12)：1260-1264,5.DOI:10.3724/SP.J.1123.2012.07031
柱前衍生化液相色谱-串联质谱法测定茶叶中草铵膦的残留量
Determination of glufosinate residue in tea by liquid chromatography-tandem mass spectrometry coupled with precolumn derivatization
摘要
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-C1) in borate buffer for 2 h. The separation was performed on a Kinetex C18 column with the mobile phases of acetoni-trile 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.关键词
柱前衍生/液相色谱-串联质谱/草铵膦/茶叶Key words
precolumn derivatization/liquid chromatography-tandem mass spectrometry (LC-MS/MS) /glufosinate/tea分类
化学化工引用本文复制引用
林永辉,刘正才,杨方,邱元进,刘素珍,苏芝娇,张琼,薛芝敏,方宇..柱前衍生化液相色谱-串联质谱法测定茶叶中草铵膦的残留量[J].色谱,2012,30(12):1260-1264,5.基金项目
国家质量监督检验检疫总局科研项目(2009IK143)和福建检验检疫局科技计划项目(FK2011-35) （2009IK143）
