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

摘要:

建立了一种利用顶空固相微萃取气相色谱法(HSSPMEGC)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， 0.02～1 000.00，0.02～1 000.00 μg·L-1；检出限分别为50，8，8 ng·L-1；加标2 μg·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.

Abstract:

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 (GCFID).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.