Synthesis and application of a T-2 toxin imprinted polymer.
Synthesis and application of a T-2 toxin imprinted polymer.
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DOI：
10.1016/j.chroma.2010.02.068
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发表时间：
2010-04
期刊：
影响因子：
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通讯作者：
David De Smet;S. Monbaliu;P. Dubruel;C. V. Van Peteghem;E. Schacht;S. de Saeger
中科院分区：
文献类型：
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作者：
David De Smet;S. Monbaliu;P. Dubruel;C. V. Van Peteghem;E. Schacht;S. de Saeger
首次报道了T-2毒素印迹聚合物的合成及其在食品分析中的应用。采用本体聚合的方法合成了一种选择性识别T-2毒素的分子印迹聚合物。甲基丙烯酰胺和乙二醇二甲基丙烯酸酯分别作为功能单体和交联剂。为进一步应用于T-2的分析，优化了分子印迹固相萃取(MISPE)程序。Scatchard图分析表明，在印迹聚合物中形成了两类印迹结合位点。高亲和力结合部位的解离常数(Kd)为7.0Mol/L，低亲和力结合部位的解离常数Kd为54.7Mol/L，并与非印迹聚合物、OASIS HLBR和免疫亲和柱的结果进行了比较。根据食物基质和添加浓度的不同，MISPE和非印迹固相萃取的回收率分别在60%到73%和21%到57%之间。用OASIS HLB®和IAC净化后的回收率分别为74-104%和60-85%。尽管OASIS HLB®吸附剂的回收率最高，但设计的MIP和IAC在选择性、交叉反应性、基质效应、检测限(LOD)和定量限(LOQ)方面都更好。根据基质的不同，MISPE后的低密度为0.4~0.6μg/kg，低密度为1.4~1.9μg/kg。清理后的LOD和LOQ分别为0.9~3.5μg/kg和3.1~11.7μg/kg。IAC测定的最低检出限和最低检出限分别为0.3~2.3μg/kg和1.0~7.7μg/kg。对39个天然污染的样品(玉米、大麦和燕麦)进行了液-质联用分析，结果表明分子印迹聚合物是清除污染食品样品的一种很好的选择。
The synthesis of a T-2 toxin imprinted polymer and its application in food analysis are reported for the first time. A molecularly imprinted polymer (MIP) for the selective recognition of T-2 toxin (T-2) was synthesized by bulk polymerization. Methacrylamide and ethyleneglycol dimethacrylate were applied as functional monomer and cross-linker, respectively. Molecularly imprinted solid-phase extraction (MISPE) procedures were optimized for further application in the analysis of T-2. Scatchard plot analysis revealed that two classes of imprinted binding sites were formed in the imprinted polymer. The dissociation constant (KD) of the higher affinity binding sites was 7.0μmol/l, while the KDof the lower affinity binding sites was 54.7μmol/l. The performance of the MIP throughout the clean-up of spiked maize, barley and oat sample extracts was compared with the results obtained when using non-imprinted polymer, OASIS HLB®and immunoaffinity columns (IAC). Depending on the food matrix and the spiked concentration, recoveries after MISPE and non-imprinted solid-phase extraction varied respectively from 60% to 73% and from 21% to 57%. Recoveries obtained after clean-up using OASIS HLB®and IAC were in the range of 74–104% and 60–85%, respectively. Although highest recoveries were obtained with OASIS HLB®sorbents, the designed MIP and the IAC were superior regarding selectivity, cross-reactivity, matrix effect, limits of detection (LOD) and limits of quantification (LOQ). Depending on the matrix, LOD after MISPE ranged from 0.4μg/kg to 0.6μg/kg and LOQ from 1.4μg/kg to 1.9μg/kg. LOD and LOQ after OASIS HLB®clean-up varied from 0.9μg/kg to 3.5μg/kg and from 3.1μg/kg to 11.7μg/kg, respectively. The LOD and LOQ values obtained with IAC were in the range of 0.3–2.3μg/kg and 1.0–7.7μg/kg, respectively. Analysis of 39 naturally contaminated samples (maize, barley and oat) by liquid chromatography tandem mass spectrometry revealed that the MIP could be an excellent alternative for clean-up of contaminated food samples.