色谱

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

• 研究论文 • 上一篇    下一篇

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

林永辉*, 刘正才, 杨方, 邱元进, 刘素珍, 苏芝娇, 张琼, 薛芝敏, 方宇   

  1. 福建出入境检验检疫局, 福建 福州 350001
  • 收稿日期:2012-07-17 修回日期:2012-09-25 出版日期:2012-12-28 发布日期:2012-12-19
  • 通讯作者: 林永辉,硕士,工程师. Tel: (0591)87065541, E-mail: xmulyh@163.com.
  • 基金资助:

    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).

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

PDF

660

被引次数

32

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2.5～50.0 μg/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。

关键词: 草铵膦, 茶叶, 液相色谱-串联质谱, 柱前衍生

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