Cacho Carmen, Schweitz Leif, Turiel Esther, Pérez-Conde Concepción
Departamento de Química Analítica, Facultad de Ciencias Químicas, Universidad Complutense de Madrid, Ciudad Universitaria s/n, 28040 Madrid, Spain.
J Chromatogr A. 2008 Feb 1;1179(2):216-23. doi: 10.1016/j.chroma.2007.11.097. Epub 2007 Dec 3.
In this work, the suitability of the combination of molecular imprinting and capillary electrochromatography (MIP-CEC) to be used as powerful tool in environmental or food analysis has been for the first time studied and successfully demonstrated. A molecularly imprinted monolith (MIM) has been synthesised and evaluated as stationary phase for the selective determination of the fungicide thiabendazole (TBZ) in citrus samples by non-aqueous capillary electrochromatography. The influence of the mobile phase composition, the voltage of the power supply and the separation temperature on the recognition of TBZ by the imprinted polymer has been evaluated, and the imprint effect in the MIM was clearly demonstrated. Once optimum recognition conditions were established, other variables affecting mechanical properties and chromatographic performance of MIM were adjusted using computational approach. The high selectivity achieved by the MIP-CEC developed procedure allowed unambiguous detection and quantification of TBZ in citrus samples by direct injection of the crude sample extracts, without any previous clean-up, in less than 6 min. The developed method was properly validated and the calculated detection limits were below the established maximum residue limits (MRLs), clearly demonstrating the suitability of the method to be used for the control of the selected fungicide.
在本研究中，首次对分子印迹与毛细管电色谱联用技术（MIP-CEC）作为环境或食品分析中强大工具的适用性进行了研究，并成功得到验证。合成了一种分子印迹整体柱（MIM），并将其作为固定相，用于通过非水毛细管电色谱法选择性测定柑橘样品中的杀菌剂噻菌灵（TBZ）。评估了流动相组成、电源电压和分离温度对印迹聚合物识别TBZ的影响，并清楚地证明了MIM中的印迹效应。一旦确定了最佳识别条件，就使用计算方法调整影响MIM机械性能和色谱性能的其他变量。所开发的MIP-CEC方法实现的高选择性使得通过直接注入粗样品提取物，无需任何预先净化，即可在不到6分钟的时间内明确检测和定量柑橘样品中的TBZ。所开发的方法经过了适当验证，计算出的检测限低于既定的最大残留限量（MRLs），清楚地证明了该方法适用于所选定杀菌剂的控制。
