超高效液相色谱-电喷雾串联质谱法测定食品包装材料中3种有机锡化合物的迁移量  

Simultaneous determination of the migration of three organotin compounds in food package material by ultra-performance liquid chromatography-electrospray tandem mass spectrometry

作　　者：许欣欣[1] 陈慧玲[1] 毛丽莎[1] 刘红河[1] 康莉[1] 

机构地区：[1]深圳市疾病预防控制中心,广东深圳518055

出　　处：《现代预防医学》2016年第11期2036-2040,共5页Modern Preventive Medicine

基　　金：深圳市卫生计生系统科研项目"食品包装材料中有机锡迁移行为研究"(No:201402073)

摘　　要：目的建立食品包装材料中三甲基锡（TMT）、三丁基锡（TBT）和三苯基锡（TPh T）迁移量的超高效液相色谱-串联质谱联用法（UPLC-MS/MS）。方法在水、10%（v/v）乙醇溶液和3%（w/v）乙酸溶液3种食品模拟物中加入0.125 mol/L盐酸溶液,使有机锡化合物呈阳离子态,经阳离子固相萃取柱净化富集,洗脱液在40℃水浴下氮气吹干;正己烷食品模拟物直接在40℃水浴下氮气吹干。残渣用流动相溶解,旋涡混匀60 s,过0.22μm微孔滤膜,经C18色谱柱分离,串联质谱仪上采用多反应监测正离子模式测定,外标法定量。结果 3种有机锡化合物在1.0-100μg/L范围内相关系数大于0.999 8,检出限为0.1-0.3μg/L。平均回收率,三甲基锡为90.6%-97.3%、三丁基锡为89.5%-94.1%,三苯基锡为88.6%-96.0%。RSD小于6.7%。结论本法快速简便、准确,可用于测定食品包装材料三甲基锡、三丁基锡和三苯基锡的迁移量。Objective To establish a method for simultaneous determination of migration of three triorganotins including trimethyltin（TMT）,tributyltin（TBT） and triphenyltin（TPh T） in food package material by ultra- performance liquid chromatography coupled with electrospray tandem mass spectrometry（UPLC- MS/MS）.Methods To make triorganotins in cationic state,0.125 mol/L hydrochloric acid solution was added to three types of food simulants including water,10%（v/v）ethanol solution and 3%（w/v） acetic acid solution.After purification and enrichment by OASIS MCX C18 cartridge,the elutes were evaporated to dryness under nitrogen flow in a 40℃ water bath,and the n- hexane simulant was evaporated to dryness directly.The residues were redissolved with 1ml of the mobile phase,vortexed for 60 s and filtered with the 0.22μm membrane.The filtrate was analyzed by UPLC- MS/MS in positive ion electrospray and MRM mode with a UPLC C18 column as a separation column and quantified with external standards.Results The linearities of the method were 1.0~100μg/L with a correlation coefficient 〉0.9998.The detection limits of the method ranged from 0.1μg/L to 0.3μg/L.The recoveries were from 88.6% to 97.3%,and the relative standard derivations（RSD） were〈 6.7%.Conclusion The method is simple,reliable and accurate,and it can be applied to the simultaneous determination of migration of TMT,TBT,and TPh T in food package material.

关 键 词：超高效液相色谱-电喷雾串联质谱 三甲基锡 三丁基锡 三苯基锡 食品包装材料 

分 类 号：R115[医药卫生—公共卫生与预防医学]