Institute of Chemistry, Department of Analytical Chemistry, University of Campinas, P.O. Box 6154, 13084-971 Campinas, SP, Brazil.
Anal Bioanal Chem. 2010 Jun;397(3):1355-61. doi: 10.1007/s00216-010-3629-4. Epub 2010 Mar 25.
A new and selective sorbent for molecularly imprinted solid-phase extraction (MISPE) was developed and applied for the determination of residues of fenitrothion (FNT) in tomatoes, using HPLC coupled to photodiode array detection (HPLC-DAD). Using FNT as the template molecule, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, toluene as the porogenic solvent, and bulk polymerization as the synthetic method, a molecularly imprinted polymer (MIP) was synthesized. In order to choose the medium which promotes the best molecular recognition of FNT by the MIP, the adsorption of FNT by the MIP was studied in different media containing acetonitrile and toluene. Besides FNT, three structurally related compounds were used to evaluate the selectivity of the FNT-molecularly imprinted polymer. The MIP exhibited the highest selective rebinding to FNT. The method developed was validated, using fortified blank tomato samples. The extraction efficiency was 96%. The limits of detection and quantitation were 0.050 and 0.130 microg g(-1), respectively. The intra-day precision was 5.9% and the inter-day precision 8.1%. The accuracy was higher than 89% for a concentration level around the maximum residue limit of 0.5 microg g(-1).
采用新的选择性分子印迹固相萃取(MISPE)吸附剂,建立了高效液相色谱-光电二极管阵列检测(HPLC-DAD)方法用于检测番茄中残留的杀螟硫磷(FNT)。以 FNT 为模板分子、甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂、甲苯为致孔剂,采用本体聚合法制备了分子印迹聚合物(MIP)。为了选择对 FNT 具有最佳分子识别能力的介质,研究了 MIP 在含乙腈和甲苯的不同介质中对 FNT 的吸附作用。除了 FNT 之外,还使用三种结构相关的化合物来评估 FNT 分子印迹聚合物的选择性。MIP 对 FNT 表现出最高的选择性再结合。使用加标空白番茄样品对所建立的方法进行了验证。该方法的提取效率为 96%。检测限和定量限分别为 0.050 和 0.130μg g(-1)。日内精密度为 5.9%,日间精密度为 8.1%。在接近最大残留限量 0.5μg g(-1)的浓度水平下,准确度高于 89%。