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  

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

作　　者：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] 

机构地区：[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

出　　处：《色谱》2014年第8期855-860,共6页Chinese Journal of Chromatography

基　　金：国家质检总局科技计划项目(2014IK090)

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3.4μg / kg（以 Sn 计），在10、20、50、200μg / 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。A method for the simultaneous determination of cyhexatin,triphenyltin and fenbuta-tin 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 monito-ring（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 simulta-neous 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.

关 键 词：格氏试剂 衍生化 气相色谱-串联质谱 三环锡 三苯锡 苯丁锡 水果 蔬菜 

分 类 号：O658[理学—分析化学]