乙基化衍生-顶空固相微萃取-气相色谱串联质谱法测定海水中的有机锡化合物  

Speciation of Organotin Compounds in Seawater by Headspace Solid Phase Microextraction and Gas Chromatography-Tandem Mass After Ethylation

作　　者：崔宗岩[1] 葛娜[1] 曹彦忠[1] 刘永明[1] 李金[1] 吴艳萍[1] 

机构地区：[1]秦皇岛出入境检验检疫局技术中心,秦皇岛066004

出　　处：《分析化学》2013年第12期1887-1892,共6页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局科技计划项目(No.2011IK197)资助

摘　　要：建立了四乙基硼化钠衍生,采用75μm聚二甲基硅氧烷/碳分子筛（PDMS/CAR）纤维进行顶空固相微萃取,结合气相色谱-三重四级串联质谱（GC-MS/MS）的检测方法,用于海水中5种机锡化合物的检测。实验流程操作简单,海水样品中加入内标三丙基锡后,使用醋酸-醋酸钠缓冲溶液调节至pH5.0,然后加入衍生试剂四乙基硼化钠,在磁力搅拌条件下进行顶空固相微萃取,萃取完成后将萃取纤维直接插入气相色谱进样口进行解析、分离和检测。日常检测单个样品的平均分析时间少于25min,而且无需有毒的有机溶剂。方法灵敏度高,对于5种有机锡化合物的检出限范围为0.10～0.20ng/L（Sn）。本方法具有良好的准确度和精密度,在20ng/L（Sn）的添加浓度下,5种有机锡化合物回收率范围为80.2%～93.6%,相对标准偏差均小于13%。所建立的方法用于渤海湾养殖区96个海水样品中有机锡化合物的检测,检出率为42.7%。A method for the determination of five organotin compounds （OTs）, monobutyltin （MBT）, dibutyltin （DBT）, tributyltin （TBT）, monophenylfin （MPhT） and diphenyhin （DPhT）, in seawater was developed using solid phase microextraction （SPME） coupled with gas chromatography and triple quadrupole tandem mass spectrometer （GC-MS/MS） after ethylation with sodium tetraethylbroate （NaBEt4 ）. After the internal standard （Tripropyltin, TPrT） was added, the pH was adjusted to 5.0 by HAc-NaAc buffer, and NaBEt4 was added, the seawater sample was stirred with a magnetic agitator and the headspace solid phase microextraction was performed with a 75 μm polydimethylsiloxane/carboxen （PDMS/CAR） fiber for 20 min. After extraction, the SPME fiber was directly injected into the GC inlet for GC-MS/MS analysis. The method has very low detection limits for the five organofin compounds in the range of 0.10-0.20 ng/L （Sn）. The recoveries are in the range of 80.2% -93.6%, and the relative standard deviations are all below 13% for the five organotin compounds at the spike level of 20 ng/L （Sn）. The method is simple, fast, sensitive and solventless. No more than 25 minutes were needed for each sample in routine analysis. The proposed method was applied to 96 seawater samples collected from mariculture areas along the Bohai Bay and the detection rate was 42.7%.

关 键 词：气相色谱串联质谱 固相微萃取 乙基化衍生 有机锡 海水 

分 类 号：O657.63[理学—分析化学] X834[理学—化学]