微波辅助提取-高效液相色谱-电感耦合等离子体质谱测定海产品中苯基锡化合物  

Determination of Phenyltin Compounds in Seafood by Microwave Assisted Extraction-HPLC-ICP-MS

作　　者：马冰峰 郭岚[2] 雷晓康[2] 柳英霞[2] 万益群[2] 

机构地区：[1]江西省产品质量监督检测院,江西南昌330029 [2]南昌大学分析测试中心,江西南昌330047

出　　处：《分析科学学报》2014年第6期858-862,共5页Journal of Analytical Science

基　　金：国家自然科学基金(No.21105043);江西省科技支撑计划项目(No.2008BB22400);食品科学与技术国家重点实验室自由探索资助项目(No.SKLF-TS-200918)

摘　　要：建立了海产品中苯基锡化合物二苯基锡、三苯基锡、四苯基锡的微波辅助提取-高效液相色谱-电感耦合等离子体质谱（MAE-HPLC-ICP-MS）分析方法。样品用丙酮-正己烷（3∶1,V/V）混合溶剂微波辅助提取,C18固相萃取小柱净化,HPLC-ICP-MS测定。在0.50-40μg/L范围内,色谱峰面积与三种苯基锡化合物浓度呈良好的线性关系（相关系数〉0.999）,检测限分别为0.16、0.11和0.18μg/L,平均加标回收率在91.2%-104%之间,相对标准偏差（RSD）〈5%。方法可应用于虾米、海砺干、蛤砺干、海星等海产品中以上三种苯基锡的同时测定。A sensitive and accurate method for the simultaneous determination of three phenyltin compounds（diphenyltin,triphenyltin and tetraphenyltin）in seafood samples by MAE-HPLC-ICP-MS has been proposed.The samples were extracted with acetone-hexane（3∶1）by MAE,then purified on a C18 solid phase extraction column and detected by HPLC-ICP-MS.The peak area was linearly valuated with the concentrations of the three compounds in the range of 0.50-40μg/L（r〉0.999）.The limits of instrument detection of DPhT,TPhT and TePhT were 0.16μg/L,0.11μg/L and 0.18μg/L,respectively.The average recoveries were in the range of 91.2%-104% with the RSDs below 5%.The proposed procedure has been applied to the determination of the three analytes in several seafood samples with satisfactory results.

关 键 词：微波辅助提取 高效液相色谱/电感耦合等离子体质谱 苯基锡 海产品 

分 类 号：O657.63[理学—分析化学]