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首页> 外文期刊>Analytica chimica acta >Use of itaconic acid-based polymers for solid-phase extraction of deoxynivalenol and application to pasta analysis
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Use of itaconic acid-based polymers for solid-phase extraction of deoxynivalenol and application to pasta analysis

机译:衣康酸基聚合物在固相萃取脱氧雪腐烯醇中的应用及其在面食分析中的应用

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Molecular modelling and computational design were used to identify itaconic acid(IA)as a functional monomer with high affinity towards deoxynivalenol(DON),a Fusarium-toxin frequently occurring in cereals.IA-based polymers were photochemically synthesised in dimethyl formamide(porogen)using ethylenglycol dimethacrylate as cross-linker and 1,1'-azo-bis(cyclohexane carbonitrile)as initiator,and the relevant binding interactions with DON in solvents with different polarity were investigated.The performances of the non-imprinted IA-based polymer(blank polymer,BP)and the corresponding molecularly imprinted polymer(MIP)were compared using DON as a template.Both BP and MIP were able to bind about 90% DON either in toluene,water or water containing 5% polyethylene glycol.Non-imprinted polymers with different molar ratios of IA to cross-linker were evaluated as adsorbents for solid-phase extraction(SPE)clean-up and pre-concentration of DON from wheat and pasta samples prior to HPLC analysis.Samples were extracted with PBS/0.1 M EDTA solution and cleaned up through a cartridge containing blank IA-based polymer.The column was washed with PBS(pH 9.2)and the toxin was eluted with methanol and quantified by reversed-phase HPLC with UV detector(gamma=220nm),using methanol:water:acetic acid(15:85:0.1,v/v/v)as the mobile phase.Effective removal of matrix interferences was observed only for pasta with DON recoveries higher than 70%(RSD<7%,n=3)at levels close to or higher than EU regulatory limit.
机译:通过分子建模和计算设计鉴定衣康酸(IA)是对谷物中常见的镰刀菌毒素,对脱氧雪腐烯(DON)具有高亲和力的功能单体.IA基聚合物是在二甲基甲酰胺(成孔剂)中光化学合成的。研究了二甲基丙烯酸乙二醇酯作为交联剂和1,1'-偶氮-双(环己烷腈)作为引发剂,以及在不同极性溶剂中与DON的相关键合作用。非印迹IA型聚合物(空白)的性能以DON为模板比较了BP和相应的分子印迹聚合物(MIP).BP和MIP都能在甲苯,水或含5%聚乙二醇的水中结合约90%DON。在HPLC分析之前,将具有不同摩尔比的IA与交联剂的IA评估为吸附剂,用于固相萃取(SPE)纯化和从小麦和面食样品中进行DON的预浓缩。用PBS / 0.1 M EDTA溶液萃取样品,并通过装有空白IA基聚合物的小柱进行纯化。用PBS(pH 9.2)洗涤色谱柱,用甲醇洗脱毒素,并通过带有HPLC的反相HPLC进行定量(γ= 220nm),以甲醇:水:乙酸(15:85:0.1,v / v / v)为流动相。只有DON回收率高于70%(RSD)的面食才能有效去除基质干扰<7%,n = 3),接近或高于欧盟法规限制。

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