Departamento de Medio Ambiente, INIA, Madrid, Spain.
J Sep Sci. 2011 Jan;34(2):217-24. doi: 10.1002/jssc.201000277.
In this work, the synthesis of molecularly imprinted polymer microspheres with narrow particle size distributions and core-shell morphology by a two-step precipitation polymerization procedure is described. Polydivinylbenzene (poly DVB-80) core particles were used as seed particles in the production of molecularly imprinted polymer shells by copolymerization of divinylbenzene-80 with methacrylic acid in the presence of thiabendazole (TBZ) and an appropriate porogen. Thereafter, polymer particles were packed into refillable stainless steel HPLC columns used in the development of an inline molecularly imprinted SPE method for the determination of TBZ in citrus fruits and orange juice samples. Under optimized chromatographic conditions, recoveries of TBZ within the range 81.1-106.4%, depending upon the sample, were obtained, with RSDs lower than 10%. This novel method permits the unequivocal determination of TBZ in the samples under study, according to the maximum residue levels allowed within Europe, in less than 20 min and without any need for a clean-up step in the analytical protocol.
在这项工作中，通过两步沉淀聚合程序描述了具有窄粒径分布和核壳形态的分子印迹聚合物微球的合成。多二乙烯基苯（poly DVB-80）核颗粒用作分子印迹聚合物壳的种子颗粒，通过在噻菌灵（TBZ）和适当的致孔剂存在下共聚二乙烯基苯-80 与甲基丙烯酸来制备。此后，将聚合物颗粒填充到可再填充的不锈钢 HPLC 柱中，用于开发用于测定柑橘类水果和橙汁样品中 TBZ 的在线分子印迹 SPE 方法。在优化的色谱条件下，根据样品的不同，TBZ 的回收率在 81.1-106.4%范围内，RSD 低于 10%。根据欧洲允许的最大残留水平，根据研究中的样品，该新方法允许在不到 20 分钟内并在分析方案中无需进行任何净化步骤的情况下，明确测定 TBZ。
