色谱Issue(10)：1090-1096,7.DOI:10.3724/SP.J.1123.2015.04045
柱前衍生-超高效液相色谱-串联质谱法同时检测茶叶中草甘膦和草铵膦的残留量
Simultaneous determination of glyphosate and glufosinate-ammonium residues in tea by ultra performance liquid chromatography-tandem mass spectrometry coupled with pre-column derivatization
摘要
Abstract
A method was developed for the determination of glyphosate( GLY)and glufosinate-ammonium( GLUF)in tea using ultra performance liquid chromatography-tandem mass spec-trometry( UPLC-MS/MS). The sample was extracted with ultrapure water and dichloromethane for 30 min under ultrasonication,followed by a simple cleanup with a C 18 solid phase extraction ( SPE)cartridge,and then GLY and GLUF were derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl)in borate buffer for 2 h. The derivatives of GLY and GLUF were separated on a Waters C18 column(50 mm×2. 1 mm,1. 7 μm)in a gradient elution mode,and finally detected with positive electrospray ionization-mass spectrometry ( ESI-MS/MS ) in multiple reaction monitoring( MRM ) mode. The quantification analysis was performed by external standard method. The method showed a good linearity( r>0. 990)in the range of 0. 003 125-0. 1 mg/L. The limits of detection( LODs)of GLY and GLUF were 0. 03 mg/kg. At the spiked levels of 0. 375,1. 5 and 4. 5 mg/kg,the recoveries of GLY and GLUF were 87. 37%-99. 11% and 81. 44%-86. 17% respectively,and the relative standard deviations( RSDs)( n=6)of GLY and GLUF were 0. 68%-1. 35% and 1. 01%-2. 33%,respectively. This method is simple,rapid and charac-terized with acceptable sensitivity and accuracy to meet the requirements for the analysis of GLY and GLUF simultaneously in tea.关键词
超高效液相色谱-电喷雾串联质谱/柱前衍生化/草甘膦/草铵膦/茶Key words
ultra high performance liquid chromatography-electrospray ionization tandem mass /spectrometry(UPLC-ESI-MS/MS)/pre-column derivatization/glyphosate(GLY)/glufosinate-ammonium( GLUF)/tea分类
化学化工引用本文复制引用
吴晓刚,陈孝权,肖海军,刘彬球..柱前衍生-超高效液相色谱-串联质谱法同时检测茶叶中草甘膦和草铵膦的残留量[J].色谱,2015,(10):1090-1096,7.基金项目
云南省企业技术中心创新能力建设项目（2009D1037）． （）
