经粉碎后的水果样品用甲醇-水(10+90)超声提取,取上清液进行离子液体-液相微萃取(IL-LPME)处理,对样品中3种有机磷农药(OPP′s)马拉硫磷、毒死蜱及对硫磷进行富集分离。采用1-丁基-3-甲基咪唑六氟硼酸盐离子液体作为萃取溶剂,与不经LPME富集分离直接进样分析相比较,经LPME操作后,上述3种OPP′s的富集倍数分别为132,119,147倍。气相色谱测定时采用HP-5毛细管色谱柱火焰光度检测器。3种农药的线性范围均在1.00~20.0 mg·L-1之间,检出限(3S/N)依次为0.4,0.1,0.2 mg·L-1。用几种水果样品作为基体,加标回收率在96.5%~104.3%之间,相对标准偏差(n=5)均小于6%。

Smashed fruit sample was extracted with CH3OH-H2O (10+90) ultrasonically, the supernatant was taken for IL-LPME treatment, to separate and enrich the 3 organophosphorus pecticides (OPP′s), namely malathion, chlorphrifos and parathion, which were determined by GC. The ionic liquid, 1-butyl-3-methylimidazole-hexafluoroborate was used as solvent for extraction. Enrichment multiples of IL-LPME were found to be 132, 119, 147 times higher than those without LPME for the 3 pesticidos respectively. HP-5 quartz capillary column was used in GC separation and flame photometric detection was adopted in the determination. Ranges of linearity for the 3 OPP′s were same between 1.00-20.0 mg·L-1, with values of detection limits (3S/N) of 0.4, 0.1, 0.2 mg·L-1 respectively. Using fruit samples as matrixes, values of recovery found by standard addition method were in the range of 96.5%-104.3% with RSD′s (n=5) less than 6%.