Guadaño-Sánchez Miriam, López Juan J, Serrano Luis A, Álvaro-Gómez Laura, Pérez Lucas, Saura-Múzquiz Matilde, Urraca Javier L
Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, 28040, Madrid, Spain.
Laboratorio de Desarrollo Analítico y Quimiometría (LADAQ), Cátedra de Química Analítica I, Facultad de Bioquímica y Ciencias Biológicas, Universidad Nacional del Litoral, Ciudad Universitaria, 3000, Santa Fe, Argentina.
Anal Bioanal Chem. 2025 Jun;417(14):3141-3156. doi: 10.1007/s00216-025-05854-8. Epub 2025 Apr 17.
A fast, accurate, and simple method of molecularly imprinted solid-phase extraction from magnetic molecularly imprinted polymers (m-MISPE) has been developed for the determination of cyclopiazonic acid (CPA) in food samples. For the synthesis of the magnetic molecularly imprinted polymers, the core-shell method through microwave irradiation was employed. Firstly, as the core halloysite nanotubes were functionalized with magnetite nanoparticles. Then, the molecular imprinted polymer (MIP) shell was created around the halloysite nanotube cores by microwave induction. In the MIP synthesis for the template molecule, an analogous compound in structure to that of CPA has been used as a surrogate molecule to reduce the costs and toxicity produced by the toxin. Besides, washing and elution m-MISPE steps were optimized to eliminate the interferences. Cross-reactivity of the m-MISPE proposed method has been tested with different mycotoxins to determine the selectivity of the polymer towards CPA (imprinting factor (IF): MIP/NIP = 3,1; MIP/NIP = 2,2; MIP/NIP = 1,7; MIP/NIP = 0,8). Finally, the m-MISPE method has been successfully applied to rice flour samples at three different concentration levels, 75, 120, and 200 μg/L, whose recoveries were 83, 97, and 93% and their RDS were 1, 2, and 2, respectively. The detection and quantification limits were 11.1 and 36.5 µg/kg respectively. This procedure is considered an easy and economical analytical way to determine CPA in food in routine laboratories of any food quality and is easy to implement versus the current methods in the determination of this mycotoxin.
已开发出一种快速、准确且简单的从磁性分子印迹聚合物（m-MISPE）中进行分子印迹固相萃取的方法，用于测定食品样品中的环匹阿尼酸（CPA）。对于磁性分子印迹聚合物的合成，采用了微波辐射下的核壳法。首先，作为核心的埃洛石纳米管被磁铁矿纳米颗粒功能化。然后，通过微波诱导在埃洛石纳米管核心周围形成分子印迹聚合物（MIP）壳。在针对模板分子的MIP合成中，一种结构与CPA类似的化合物被用作替代分子，以降低毒素产生的成本和毒性。此外，对m-MISPE的洗涤和洗脱步骤进行了优化以消除干扰。已用不同的霉菌毒素测试了所提出的m-MISPE方法的交叉反应性，以确定该聚合物对CPA的选择性（印迹因子（IF）：MIP/NIP = 3.1；MIP/NIP = 2.2；MIP/NIP = 1.7；MIP/NIP = 0.8）。最后，m-MISPE方法已成功应用于三种不同浓度水平（75、120和200 μg/L）的米粉样品，其回收率分别为83%、97%和93%，相对标准偏差分别为1%、2%和2%。检测限和定量限分别为11.1和36.5 µg/kg。该方法被认为是在任何食品质量的常规实验室中测定食品中CPA的一种简便且经济的分析方法，并且与目前测定这种霉菌毒素的方法相比易于实施。
