基于分子印迹富集及HPLC-ICP-MS检测海产品中三丁基锡的研究

Determination of Trace Tributyltin in Seafood by Molecularly Imprinted Polymer and High Performance Liquid Chromatography-inductively Coupled Plasma Mass Spectrometry

摘要:

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0.06 μg/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0.1 μg/L~30 μg/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。

Abstract:

With methacrylate as functional monomer, tributyltin (TBT) as template molecule, ethylene glycol dimethyl ester as crosslinking agent, and acetonitrile as porogen, a molecularly imprinted polymer (MIP) with specific recognition towards TBT was successfully prepared using molecular imprinting technology combined with high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). Experiments on selective recognition, adsorption kinetics, and regeneration performance showed that the synthesized MIPS had a good adsorption capacity and high selective recognition ability for TBT. Additionally, MIPs were used as solid phase extraction sorbents to separate and enrich TBT, and the TBT in seawater and seafood was detected using HPLC-ICP-MS. The results indicated that, compared with traditional MIPs as an adsorbent for enrichment and separation, the limits of detection (LODs) for seawater, mussels, and large yellow croaker samples were 0.06 μg/L, 4.0 ng/g, and 5.0 ng/g, respectively, the recoveries were 61.5%~84.5%, 76.2%~93.9%, and 74.2%~93.3%, respectively, and the linear ranges were 0.1 μg/L~30 μg/L, 5 ng/g~50 ng/g, and 5 ng/g~500 ng/g, respectively. This study provides a method for the detection of organic tin and other organometallic compounds in seafood.