基于磁性分子印迹联用高效液相色谱-电感耦合等离子体质谱测定海产品中的三丁基锡
Determination of tributyltin in seafood based on magnetic molecularly imprinted polymers coupled with high performance liquid chromatography-inductively coupled plasma mass spectrometry
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摘要: 以四氧化三铁作为支撑体进行表面分子印迹,通过两步聚合,在其表面修饰上功能单体(甲基丙烯酸MAA),与模板分子(三丁基锡TBT)、交联剂(二甲基丙烯酸乙二醇酯EGDMA)和致孔剂(乙腈)聚合,成功地制备了能特异性识别TBT的磁性分子印迹聚合物(Fe3O4@MIPs)。对其进行物理表征,并研究了其吸附、选择等能力。结果表明,该磁性分子印迹聚合物对比传统印迹聚合物有更大的吸附量,更显著的选择吸附性,而因其磁性分离特性,前处理过程变得更简易,快速。用磁性分子印迹聚合物作为吸附剂富集分离,在多种海产样品中的检测限为1.0 ng/g,加标回收率是79.74%95.72%,线性范围是5 ng/g到1000 ng/g。对贻贝、泥蚶和大黄鱼进行并联合高效液相色谱电感耦合等离子质谱(HPLC-ICP-MS)分析,样品加标回收率范围在79.74%95.72%,RSD(相对标准偏差)在1.3%4.7%。该方法总分析时间更短,检测限更低,线性范围更宽,能更好地应用于海水和海产品中三丁基锡的测定。Abstract: Iron oxide as a support surface imprinting,by two- stage polymerization,surface modification on its functional monomer( MAA),and the template molecule( TBT),a crosslinking agent( EGDMA) and porogen( acetonitrile) polymerization. Research specifically recognize TBT magnetic molecularly imprinted polymer prepared successfully(Fe_3O_4@ MIPs).Its physical was be characterization,and its adsorption capacity was be selection.The results showed that the Magnetic molecularly imprinted polymer compared to traditional imprinted polymers had a greater adsorption capacity,significantly more selective adsorption,magnetic separation and because of its characteristics,the pre-treatment process became easier and faster.Magnetic molecularly imprinted polymer as an adsorbent enrichment and separation,in a variety of seafood sample detection limit of 1.0 ng / g,and the recovery was 79.74% ~ 95.72%,the linear range of 5 ng / g to 1000 ng / g. Mussels,cockles and large yellow croaker were mud and HPLC- ICP- MS analysis,sample recoveries in the range of 79.74% ~ 95.72%,RSD 1.3% ~4.7%. The method of total analysis time was shorter,lower detection limit,wider linear range,could be better applied to the determination of seawater and seafood tributyltin.