色谱2012，Vol.30Issue(6)：555-559,5.DOI:10.3724/SP.J.1123.2012.01034
液相色谱-串联质谱法测定黄瓜和苹果中氟啶虫酰胺及其代谢产物残留量
Simultaneous determination of flonicamid and its metabolites in cucumbers and apples by liquid chromatography-tandem mass spectrometry
摘要
Abstract
A method was developed for the simultaneous determination of flonicamid and its metabolite [N-(4-trifluoromethylnicotinoyl) glycine ( TFNG ), 4-trifluoromethylnicotinic acid (TFNA) and 4-trifluoromethylnicotinamide (TFNA-AM) ] in cucumbers and apples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with liquid-liquid extraction. The sample was extracted twice with phosphate buffer solution (pH 7. 0), and the extract was adjusted to pH 1.5 -2. 0, then an aliquot of the extract (3 mL) was extracted with ethyl acetate. The final extract was dried under nitrogen and the residue was dissolved in 0. 1% formic acid in water/methanol (80/20, v/v). The sample was analyzed by LC-MS/MS and quantified with the external standard calibration curve method. The detection limits of flonicamid, TFNG, TFNA and TFNA-AM were 0. 17, 0. 20, 0. 35 and 0. 60μg/kg, respectively. The average recoveries of flonicamid and its metabolites in cucumbers and apples were 82. 9% - 104. 1%. In the intra-assay, the relative standard deviations were 3. 6% - 6. 9% at the spiked levels of 5. 0 -2 000 μg/kg. There were good linear correlations (the calibration coefficients were above 0. 998) between the peak areas and the concentrations of flonicamid and its metabolites in the range of 0. 5 - 200μg/L. The volume of organic solvent used in the whole pretreatment procedure was only 6 mL. The method is accurate, highly sensitive and stable for the determination of flonicamid and its metabolites.关键词
液相色谱-串联质谱/氟啶虫酰胺/代谢产物/残留分析/黄瓜/苹果Key words
liquid chromatography-tandem mass spectrometry(LC-MS/MS)/flonicamid/metabolite/ residue analysis/ cucumbers/ apples分类
化学化工引用本文复制引用
陈国,孙亚米,杨挺,吴银良..液相色谱-串联质谱法测定黄瓜和苹果中氟啶虫酰胺及其代谢产物残留量[J].色谱,2012,30(6):555-559,5.基金项目
宁波市自然科学基金项目(No.2009A610183)和宁波市农业攻关项目(No.2010C10029和2010C10026). （No.2009A610183）
