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本文以甲基丙烯酸为功能单体,三丁基锡为模板分子,二甲基丙烯酸乙二醇酯为交联剂,乙腈为致孔剂,采用分子印迹技术并联合高效液相色谱电感耦合等离子质谱(HPLC-ICP-MS)成功地制备了能特异性识别TBT的MIPs。所合成的MIPS经过选择识别、吸附动力学及再生性能等检测,对三丁基锡具有良好的吸附能力和高选择识别能力。并以分子印迹聚合物作为固相萃取吸附剂分离富集TBT,联合高效液相色谱-电感耦合等离子质谱(HPLC-ICP-MS)检测海水及海产品中的三丁基锡。结果表明,用传统分子印迹聚合物作为吸附剂富集分离,在海水、贻贝和大黄鱼样品中检测限(LOD)分别为0.06μg/L、4.0 ng/g和5.0 ng/g,加标回收率分别是61.5%~84.5%、76.2%~93.9%和74.2%~93.3%,线性范围分别是0.1μg/L~30μg/L、5 ng/g~50 ng/g和5 ng/g~500 ng/g。为海产品中有机锡等有机金属的检测提供方法。
In this paper, methacrylic acid as a functional monomer, tributyltin as a template molecule, ethylene glycol dimethacrylate as a cross-linking agent, acetonitrile porogen, molecular imprinting technology and high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry ( HPLC-ICP-MS) successfully prepared MIPs that specifically recognize TBT. The synthesized MIPS through the choice of identification, adsorption kinetics and regeneration performance testing, tributyltin has good adsorption capacity and high selection of recognition. TBT was separated and enriched with molecularly imprinted polymer as solid-phase extraction adsorbent, and tributyltin in seawater and seafood was detected by HPLC-ICP-MS. The results showed that the limit of detection (LOD) was 0.06μg / L, 4.0 ng / g and 5.0 ng / g respectively in the samples of seawater, mussel and big yellow croaker by using traditional molecularly imprinted polymer as adsorbent. The recoveries were in the range of 61.5% -84.5%, 76.2% -93.9% and 74.2% -93.3%, respectively. The linear range was from 0.1μg / L to 30μg / L, 5ng / 500 ng / g. Methods for the detection of organotin and other organic metals in seafood.