离子液体液相微萃取-气相色谱法测定水果中3种有机磷农药残留  

GC Determination of Residual Amounts of 3 Organophosphorus Pesticides in Fruits with Ionic Liquid-Liquid Phase Micro-extraction(IL-LPME)

作　　者：林海禄[1,2] 彭雪娇[2] 闫红[1] 

机构地区：[1]北京工业大学生命科学与生物工程学院,北京100124 [2]东华理工大学化学生物与材料科学学院,抚州344000

出　　处：《理化检验（化学分册）》2011年第12期1440-1442,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江西省自然科学基金(2007GZH2162);江西省教育厅青年基金(GJJ 09523)

摘　　要：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1.00～20.0mg.L-1之间,检出限(3S/N)依次为0.4,0.1,0.2mg.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%.

关 键 词：气相色谱 离子液体 液相微萃取 有机磷农药 水果 

分 类 号：O657.7[理学—分析化学]