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建立了快速溶剂萃取-固相萃取柱净化-高效液相色谱法(ASE-SPE-HPLC)同时测定蔬菜中痕量双甲脒、久效磷、水胺硫磷、多效唑、克线磷、2,4-D和噻嗪酮7种农药残留量的方法。采用快速溶剂萃取仪提取样品,提取液经固相萃取柱净化后,以70%甲醇+10%乙腈+20%水为流动相,以保留时间定性确证,峰面积外标法进行定量。7种农药的浓度与其峰面积在30～360μg/L的范围内呈良好的线性关系,检出限为0.003～0.024μg/g,样品的加标平均回收率为96.3%～110%,相对标准偏差2.1%～4.8%。方法适用于蔬菜中7种农药的同时分析。
A rapid solvent extraction-solid phase extraction column and high performance liquid chromatography (ASE-SPE-HPLC) was developed for the simultaneous determination of trace amitraz, monocrotophos, acetaminophen, paclobutrazol, , 4-D and buprofezin 7 pesticide residues. The samples were extracted by fast solvent extraction. The extracts were purified by solid phase extraction (SPE) column with 70% methanol + 10% acetonitrile + 20% water as mobile phase. The retention time was qualitatively confirmed and the peak area was determined by external standard method. The concentration of seven pesticides showed a good linear relationship with the peak area of 30 ~ 360μg / L, the detection limit was 0.003 ~ 0.024μg / g, the average recovery rate of samples was 96.3% ~ 110%, the relative standard Deviations of 2.1% to 4.8%. The method is suitable for the simultaneous analysis of seven pesticides in vegetables.