液相色谱-质谱法对电子电气产品塑料部件中有机锡的测定  

Determination of Organotin Compounds in Plastic Components of Electrical and Electronic Products by Liquid Chromatography-Mass Spectrometry

作　　者：徐琴[1] 牛增元[1] 叶曦雯[1] 孙银峰[1] 汤志旭[1] 

机构地区：[1]山东出入境检验检疫局技术中心,山东青岛266002

出　　处：《分析测试学报》2009年第11期1270-1274,共5页Journal of Instrumental Analysis

基　　金：科技部"十一五"国家科技支撑计划项目资助(2006BAK04A10);2007年国家质检公益性行业科研专项基金资助(10-66)

摘　　要：建立了液相色谱-质谱法同时测定电子电气产品塑料部件中3种有机锡的方法。样品经四氢呋喃溶解，并经甲醇沉淀杂质后，用液相色谱-质谱仪进行测定和确证。色谱柱为ZORBAX 300-SCX柱（250mm×4．6mm×5μm i．d．），流动相为体积比80：20的甲醇-20mmol/L醋酸铵（含0．01％冰乙酸），等度洗脱，流速为1．0mL／min，选择离子监测模式。三丁基锡、三苯基锡、三辛基锡的线性范围分别为0．1～10．0、0．1～10．0、0．05～5．0mg／L（相关系数r^2≥0．9992），方法定量下限（LOQ）依次为0．005％、0．005％、0．0025％；平均加标回收率为80％～100％，相对标准偏差为1．6％～11．5％（n=6）。A new high performance liquid chromatography -mass spectrometric（ HPLC -MS） method was developed for the determination of 3 organotin compounds including tributyltin（TBT） , triphenyltin（TPhT） and trioctyhin（TOT） in plastic components of electrical and electronic products. Plastic samples were dissolved by tetrahydrofuran and cleaned up using impurities precipitation with methanol. The separation was performed in the isocratic mode on a ZORBAX 300-SCX column with a mobile phase containing 0. 01% glacial acetic acid in methanol-20 mmol/L ammonium acetate（80 ： 20, by volume）. The optimum HPLC -MS conditions were established and the MS system was operated by selective ion monitoring（SIM） under positive mode electrospray ionization（ESI）. Quantification was performed on the basis of [ M ] ＋ ions. The calibration curves（r^2 ≥0. 999 2） were linear over the concentration in the range of 0. 05 - 5.0 mg/L for TOT and 0. 1 - 10.0 mg/L for TBT and TPhT. The limits of quantitations（LOQ） of TBT, TPhT and TOT were 0. 005% , 0. 005% and 0. 0025% , respectively. The spiked recoveries ranged form 80% to 100% with relative standard deviations（RSDs） from 1.6% to 11.5% （n =6）. The method has merits of simplicity, sensitivity and rapidity, and could be used for simultaneous determination of organotins in plastic samples.

关 键 词：有机锡 电子电气产品 塑料 液相色谱-质谱法 

分 类 号：O657.63[理学—分析化学]