色谱

色谱 ›› 2014, Vol. 32 ›› Issue (8): 855-860.DOI: 10.3724/SP.J.1123.2014.04031

• 研究论文 • 上一篇    下一篇

格氏试剂衍生-气相色谱-串联质谱法同时测定水果和蔬菜中的三环锡、三苯锡和苯丁锡残留

崔宗岩1, 孙扬2, 葛娜1, 张进杰1, 刘永明1, 李阿丹2, 曹彦忠1   

  1. 1. 秦皇岛出入境检验检疫局检验检疫技术中心, 河北 秦皇岛 066004;
    2. 燕山大学环境与化学工程学院, 河北 秦皇岛 066004
  • 收稿日期:2014-04-18 修回日期:2014-06-25 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 曹彦忠，E-mail：caoyzciq@126.com
  • 基金资助:

    国家质检总局科技计划项目（2014IK090）.

Simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide residues in fruits and vegetables by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry

CUI Zongyan1, SUN Yang2, GE Na1, ZHANG Jinjie1, LIU Yongming1, LI Adan2, CAO Yanzhong1   

  1. 1. Qinhuangdao Entry-Exit Inspection and Quarantine Bureau, Qinhuangdao 066004, China;
    2. School of Environmental and Chemical Engineering, Yanshan University, Qinhuangdao 066004, China
  • Received:2014-04-18 Revised:2014-06-25 Online:2014-08-08 Published:2014-08-01

PDF

401

被引次数

12

摘要：

建立了水果和蔬菜中三环锡、三苯锡和苯丁锡同时检测的格氏试剂衍生-气相色谱-串联质谱方法（GC-MS/MS）。样品经盐酸/四氢呋喃（1：10，v/v）消解，正己烷振荡提取，乙基溴化镁衍生和Florisil固相萃取净化，采用GC-MS/MS多反应监测（MRM）模式对3种有机锡化合物进行定性和定量分析。实验结果表明，以苹果为代表性样品基质，三环锡、三苯锡和苯丁锡的检出限（LOD）分别为2.0、1.5和3.4 μg/kg （以Sn计），在10、20、50、200 μg/kg （以Sn计）共4个添加水平下的平均回收率为72.4%~107.1%，相对标准偏差为0.4%~14.2%。该方法灵敏度高，选择性强，可以实现3种有机锡农药的同时检测，能够满足国内外残留限量的检测要求。

关键词: 苯丁锡, 格氏试剂, 气相色谱-串联质谱, 三苯锡, 三环锡, 蔬菜, 水果, 衍生化

Abstract:

A method for the simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide residues in fruits and vegetables was developed by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). The samples were firstly digested by HCl/THF (1:10, v/v), then extracted by hexane and followed by the derivatization with Grignard reagent (EtMgBr). Then after purification using florisil SPE columns, the sample extracts were finally analyzed by GC-MS/MS. The qualitative and quantitative determinations of the three organotin pesticides were performed by the tandem mass in multiple reaction monitoring (MRM) mode. By using apple as a representative matrix, the limits of detection (LODs) obtained by the proposed method for cyhexatin, triphenyltin and fenbutatin oxide were 2.0, 1.5 and 3.4 μg/kg (as Sn), respectively. The average recoveries for the three organotin pesticides were in the range of 72.4%-107.1% at the spiked levels of 10, 20, 50 and 200 μg/kg (as Sn) and the relative standard deviations (RSDs) ranged from 0.4% to 14.2%. The proposed method was validated to have good linearity, high sensitivity, selectivity and accuracy for the simultaneous determination of cyhexatin, triphenyltin and fenbutatin oxide in fruits and vegetables. The sensitivity of this method can meet the requirements of the inspection for the three organotin pesticides at the level of maximum residue limits (MRLs) set by China and some other countries.

Key words: cyhexatin, derivatization, fenbutatin oxide, fruits, gas chromatography-tandem mass spectrometry (GC-MS/MS), Grignard reagent, triphenyltin, vegetables

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