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衣康酸基聚合物用于脱氧雪腐镰刀菌烯醇的固相萃取及其在面食分析中的应用。

Use of itaconic acid-based polymers for solid-phase extraction of deoxynivalenol and application to pasta analysis.

作者信息

Pascale Michelangelo, De Girolamo Annalisa, Visconti Angelo, Magan Naresh, Chianella Iva, Piletska Elena V, Piletsky Sergey A

机构信息

Institute of Sciences of Food Production (ISPA), National Research Council (CNR), Via G. Amendola 122/O, 70126 Bari, Italy.

出版信息

Anal Chim Acta. 2008 Feb 25;609(2):131-8. doi: 10.1016/j.aca.2008.01.004. Epub 2008 Jan 10.

Abstract

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/0.1M 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 (lambda=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.

摘要

利用分子建模和计算设计确定衣康酸(IA)是一种对脱氧雪腐镰刀菌烯醇(DON)具有高亲和力的功能单体,DON是谷物中常见的一种镰刀菌毒素。以IA为基础的聚合物在二甲基甲酰胺(致孔剂)中通过光化学合成,使用乙二醇二甲基丙烯酸酯作为交联剂,1,1'-偶氮双(环己烷甲腈)作为引发剂,并研究了其在不同极性溶剂中与DON的相关结合相互作用。以DON为模板,比较了非印迹IA基聚合物(空白聚合物,BP)和相应的分子印迹聚合物(MIP)的性能。BP和MIP在甲苯、水或含5%聚乙二醇的水中均能结合约90%的DON。评估了具有不同IA与交联剂摩尔比的非印迹聚合物作为吸附剂用于固相萃取(SPE)净化和在HPLC分析之前从小麦和面食样品中预富集DON。样品用PBS/0.1M EDTA溶液萃取,并通过装有空白IA基聚合物的柱进行净化。柱先用PBS(pH 9.2)洗涤,毒素用甲醇洗脱,并用带有紫外检测器(λ=220nm)的反相HPLC进行定量,使用甲醇:水:乙酸(15:85:0.1,v/v/v)作为流动相。仅在面食中观察到有效去除基质干扰,在接近或高于欧盟监管限值的水平下,DON回收率高于70%(RSD<7%,n=3)。

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