| 分子印迹-基质固相分散萃取-高效液相色谱法测定土壤中4种硫代磷酸酯类农药残留量 |
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| 引用本文： | 周梦春,何海,舒耀皋,舒少华,王沫.分子印迹-基质固相分散萃取-高效液相色谱法测定土壤中4种硫代磷酸酯类农药残留量[J].农药学学报,2015,17(1):83-88. |
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| 作者姓名： | 周梦春 何海 舒耀皋 舒少华 王沫 |
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| 作者单位： | 1.华中农业大学 植物科学技术学院, 武汉 430070 |
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| 摘 要： | 建立了一种高效、选择性强的分子印迹-基质固相分散萃取结合高效液相色谱测定土壤中4种硫代磷酸酯类农药(毒死蜱、甲基立枯磷、甲基毒死蜱、甲基对硫磷)残留量的方法;并以甲基立枯磷为模板分子,以甲基丙烯酸(MAA)为功能单体,且n(模板分子)∶n(功能单体)=1∶4,以乙二醇二甲基丙烯酸酯(EDMA)为交联剂,以偶氮二异丁腈为引发剂,采用沉淀印迹聚合方法,合成了甲基立枯磷高分子印迹聚合微球(MIPs);以MIPs作为土壤样品提取液的基质固相分散吸附剂,采用HPLC检测处理后的样品,流动相为V(乙睛)∶V(0.1%乙酸水溶液)=3∶1,流速0.8 m L/min,进样量20μL,检测波长210 nm,采用Agilent Eclipse XDB-C8色谱柱(150 mm×4.6 mm,5μm),柱温25℃。结果显示:MIPs对甲基立枯磷有特异性吸附,对其结构相似物毒死蜱、甲基对硫磷和甲基毒死蜱也具有一定的吸附性能;在0.01~5.0 mg/kg范围内,各药剂的质量浓度与相应的峰面积间呈良好的线性关系,相关系数r为0.997 5~0.999 8;4种硫代磷酸酯类有机磷杀虫剂的检出限(LOD)为0.452~1.226μg/kg;添加回收率为76%~96%,相对标准偏差(RSD)为2.8%~7.3%。该方法可用于土壤中硫代磷酸酯类有机磷杀虫剂残留量的测定。
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| 关 键 词： | 分子印迹聚合物 固相分散萃取 高效液相色谱 硫代磷酸酯类农药 土壤 残留 |
| 收稿时间： | 2014/6/27 0:00:00 |
| 修稿时间： | 2014/10/31 0:00:00 |
Determination of four phosphorothioate pesticide residues in soil samples by molecularly imprinted matrix solid-phase dispersion combined with high performance liquid chromatography |
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| Zhou Mengchun,He Hai,Shu Yaogao,Shu Shaohua and Wang Mo.Determination of four phosphorothioate pesticide residues in soil samples by molecularly imprinted matrix solid-phase dispersion combined with high performance liquid chromatography[J].Chinese Journal of Pesticide Science,2015,17(1):83-88. |
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| Authors: | Zhou Mengchun He Hai Shu Yaogao Shu Shaohua and Wang Mo |
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| Institution: | 1.College of Plant Science and Technology, Huazhong Agricultural University, Wuhan 430070, China2.Shanghai Research Institute of Chemical Industry, Shanghai 200062, China |
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| Abstract: | An effective and selective method for sample pretreatment, namely molecularly imprinted matrix solid-phase dispersion coupled with high performance liquid chromatography(HPLC), was developed for rapid determination of four phosphorothioate pesticides(tolclophos-methyl, chlorpyrifos, parathion-methyl, chlorpyriphos-methyl) in soil samples. New molecularly imprinted polymer microspheres(MIPs) were synthesized with precipitation blotting polymerization by using structural analogue tolclofos-methyl as template molecule and employing methacrylic acid(MAA) and ethylene glycol dimethacrylate(EDMA) as the functional monomer and cross-linker agent, and azodiisobutyronitrile as initiator. Furthermore, the molar ratio of template to functional monomer was at 1:4 in this experiment. The results indicated that the MIPs showed a special binding ability for the template and some absorbability to three other phosphorothioate pesticides(chlorpyrifos, parathion-methyl, chlorpyriphos-methyl). The obtained MIPs was used to extract and preconcentrate four phosphorothioates as adsorbent of matrix solid phase dispersion from extracting solution of soil, then the samples were detected by HPLC. The optimized method parameters were as follows: acetonitrile and pure water including 0.1% acetic acid(V/V=3/1) were selected as mobile phase, flow rate was 0.8 mL/min, sample injection voplume was 20 μL, UV detecting wavelength was 210 nm, and Eclipse XDB-C8 column(150 mm×4.6 mm,5 μm)was used as separating column with column temperature of 25 ℃. The linear correlation was 0.997 5-0.999 8 between concentrations range of 0.01-5.0 mg/kg. The detection limit of the method was 0.452-1.226 μg/kg in soil samples. With relative standard deviations of 2.8%-7.3% in soil samples, the fortified tests showed recovery rates were in the range of 76%-96% in soil samples. This study indicated that the proposed method could meet the requirements for simultaneously determinationg of phosphorothioate pesticide residues in soil. |
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| Keywords: | molecularly imprinted polymers(MIPs) dispersive solid phase extraction high performance liquid chromatography phosphorothioate pesticide soil residue |
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