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目的建立基于1-丁基-3-甲基咪唑六氟磷酸盐[Bmim][PF6]的离子液体-分散液相微萃取样品前处理技术,结合高效液相色谱同时测定蔬菜中杀扑磷、马拉硫磷、甲基对硫磷、三唑磷、杀螟硫磷、对硫磷、甲基嘧啶磷、辛硫磷和丙溴磷的方法。方法取适量匀浆样品加水定容,再减压抽滤,滤液离心后取上清液,用[Bmim][PF6]萃取(乙腈为分散剂),形成的水/分散剂/萃取剂白色乳状混浊体系经离心后,取聚集相液滴进样高效液相色谱分析。结果方法线性相关系数r>0.9991;检出限为0.0012 mg/kg~0.0110 mg/kg(S/N=3);相对标准偏差RSD<3.57%(n=7);回收率为75.0%~104.7%。结论本法简便快速、灵敏准确、萃取效率高、有机溶剂消耗少,适合蔬菜中9种农药的同时测定。
OBJECTIVE To establish an ionic liquid-dispersive liquid-phase microextraction (SPE) sample pretreatment technique based on 1-butyl-3-methylimidazolium hexafluorophosphate [Bmim] [PF6], and simultaneous determination of trimethoprim in vegetables by high performance liquid chromatography Malathion, methyl parathion, triazophos, fenitrothion, parathion, methylpyrimidine, phoxim, and profenofos. Methods The appropriate amount of homogenized sample was subjected to constant volume watering and suction filtration under reduced pressure. After the filtrate was centrifuged, the supernatant was taken and extracted with [Bmim] [PF6] (acetonitrile as dispersant) to form a water / dispersant / extractant white milky After the turbidity system was centrifuged, the aggregated phase droplet was taken for high performance liquid chromatography analysis. Results The linear correlation coefficient was 0.9991. The detection limit was 0.0012 mg / kg to 0.0110 mg / kg (S / N = 3). The relative standard deviation was less than 3.57% (n = 7) and the recovery was 75.0% -104.7 %. Conclusion The method is simple, rapid and sensitive, accurate in extraction, high in extraction efficiency and less in consumption of organic solvents. It is suitable for the simultaneous determination of nine pesticides in vegetables.