College of Chemistry, Jilin University, Changchun 130012, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Jun 15;929:27-32. doi: 10.1016/j.jchromb.2013.01.036. Epub 2013 Feb 24.
A simple, rapid and sensitive method for simultaneous determination of three N-methylcarbamate pesticides (carbaryl, pirimicarb, and isoprocarb) in vegetables was developed by coupling polymer monolith microextraction (PMME) to high-performance liquid chromatography (HPLC). A poly(methacrylic acid-co-ethylene glycol dimethacrylate) monolith was selected as the extraction medium for PMME. To achieve optimum extraction performance, several parameters were investigated, including desorption solvent, desorption flow rate, sample flow rate, sample volume, sample pH values, inorganic salt and organic solvent content of the sample solution. Under the optimum experimental conditions, the method provides an acceptable linearity (5-5000μg/kg), low limits of detection (0.36-2.6μg/kg), good precision (intra-day relative standard deviations<2.53%, inter-day relative standard deviations <6.36%). Finally, the developed method was successfully applied to the determination of N-methylcarbamate pesticides in vegetables, and the trueness was evaluated by recovery experiments. The obtained relative recoveries were in the range of 70.4-98.5%. This PMME method integrates sample extraction, purification, and preconcentration of analytes into one single step and it also has several advantages such as solvent-free extraction, small sample volume, high enrichment, convenience, and flexibility operation.
建立了一种聚合物整体柱微萃取-高效液相色谱联用测定蔬菜中 3 种 N-甲基氨基甲酸酯类农药(西维因、抗蚜威、异丙威)残留的分析方法。采用聚(甲基丙烯酸-co-乙二醇二甲基丙烯酸酯)整体柱作为萃取介质。为了获得最佳萃取性能,考察了多种参数,包括洗脱溶剂、洗脱流速、样品流速、样品体积、样品 pH 值、样品溶液中的无机盐和有机溶剂含量。在最佳实验条件下,该方法具有良好的线性(5-5000μg/kg)、低检测限(0.36-2.6μg/kg)、良好的精密度(日内相对标准偏差<2.53%,日间相对标准偏差<6.36%)。最后,将所建立的方法成功应用于蔬菜中 N-甲基氨基甲酸酯类农药残留的测定,并通过加标回收实验评估了方法的准确性。获得的相对回收率在 70.4%-98.5%之间。该整体柱微萃取方法将样品的提取、净化和浓缩集于一步完成,具有无溶剂萃取、小体积样品、高富集倍数、操作简便、灵活等优点。