顶空固相微萃取-气相色谱法测定海水中丁基锡  

Determination of Butyltin Compounds in Seawater by Headspace-solid-phase Microextraction-gas Chromatography

作　　者：朱仲良[1] 焦金红[1] 柴晓兰[1] 施踏青[1] 

机构地区：[1]同济大学化学系,上海200092

出　　处：《同济大学学报（自然科学版）》2010年第9期1324-1328,共5页Journal of Tongji University:Natural Science

摘　　要：建立了一种利用顶空固相微萃取-气相色谱法（HS-SPME-GC）检测海水中3种丁基锡化合物（一丁基锡、二丁基锡、三丁基锡）的方法.在优化实验条件时,选取缓冲溶液的pH值、缓冲溶液体积、平衡时间、萃取时间、萃取温度等5个因素进行L16（45）正交试验设计.结果表明,一丁基锡、二丁基锡、三丁基锡的线性范围分别为0.05~1 000.00,0.02~1 000.00,0.02~1 000.00μg.L-1;检出限分别为50,8,8ng.L-1;加标2μg.L-1时,回收率分别为106%,89%,91%.将该方法用于涉及中国4大海域的深圳、上海、连云港、青岛、大连、烟台等6个沿海城市近海海水样品的测定,除了青岛海滨水样外,其他5个城市海水样中均检测出了不同质量浓度的有机锡.A method for simultaneous determination of three organotin compounds named monobutyltin（MBT）,dibutyltin（DBT）,tributyltin（TBT） in seawater sample was described.The method was based on derivatization with sodium tetraethylborate followed by headspaced-solid-phase microextraction（SPME） combined with gas chromatography-flame ionization detector（GC-FID）.The SPME conditions were optimized using experimental designs（five factors and for levels）.The calibration ranges of MBT,DBT and TBT are 0.05~1 000 μg·L-1,0.02~1 000 μg·L-1,0.02~1 000 μg·L-1（as Sn）.The detection limits of MBT,DBT and TBT are 50,8,8 ng·L-1（as Sn）.The recoveries of MBT,DBT and TBT are 106%,89%,91% by analyzing seawater spiked with organotin compounds.Six samples taken from six cities（Shenzhen,Shanghai,Lianyungang,Qingdao,Dalian,Yantai） were analyzed,and organotin compounds were detected in all five samples but Qingdao.

关 键 词：丁基锡 衍生化 正交试验设计 顶空固相微萃取-气相色谱法 

分 类 号：X502[环境科学与工程—环境工程]