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

作　　者：林永辉[1] 刘正才[1] 杨方[1] 邱元进[1] 刘素珍[1] 苏芝娇[1] 张琼[1] 薛芝敏[1] 方宇[1] 

机构地区：[1]福建出入境检验检疫局,福建福州350001

出　　处：《色谱》2012年第12期1260-1264,共5页Chinese Journal of Chromatography

基　　金：国家质量监督检验检疫总局科研项目(2009IK143);福建检验检疫局科技计划项目(FK2011-35)

摘　　要：建立了茶叶中草铵膦残留检测的液相色谱-串联质谱分析方法。样品经水超声提取,C18固相萃取小柱净化,9-芴基氯甲酸酯(FMOC-Cl)溶液在硼酸盐缓冲溶液下衍生2 h后,用Kinetex C18色谱柱分离,以乙腈和5 mmol/L乙酸铵水溶液(含0.2%(v/v)甲酸)作为流动相进行梯度洗脱,电喷雾负离子模式电离(ESI-),多反应监测(MRM)模式检测,外标法定量。方法的线性范围为2.5～50.0μg/L,相关系数r2大于0.999;定量限为0.10 mg/kg。在不同基质中,草铵膦在0.10、0.50、1.00 mg/kg添加水平下的平均回收率为61.6%～81.4%,相对标准偏差为3.2%～8.4%。该方法具有快速简便、灵敏度高、准确性强等特点,适用于茶叶中草铵膦残留量的检测。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 r20.999.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 

分 类 号：O658[理学—分析化学]