title: Simultaneous determination of amitraz and its metabolite residue in food animal tissues by gas chromatography-electron capture detector and gas chromatography-mass spectrometry with accelerated solvent extraction.
abstract: A new method has been developed for determination and confirmation of amitraz and its main metabolite, 2,4-dimethylaniline, in food animal tissues using gas chromatography-electron capture detector (GC-ECD) and gas chromatography-mass spectrometry detector (GC-MS). This method is based on a new extraction procedure using accelerated solvent extraction (ASE). It consists of an n-hexane/methanol extraction step, a cleaning-up step by BakerBond octadecyl C(18) silica bonded cartridge, hydrolysis and derivatization to 2,4-dimethyl-7-F-butyramide for GC-ECD analysis. For confirmation using GC-MS, hydrolysis and derivatization were not needed. Parameters for extraction pressure, temperature and cycle of ASE, clean-up, derivatization and analysis procedure have been optimized. Spike recoveries from 50 to 300 microg/kg levels were found to be between 72.4 and 101.3% with relative standard deviation less than 11.5% in GC-ECD, from 5 to 20 microg/kg levels were found to be between 77.4 and 107.1% with relative standard deviation less than 11.6% in GC-MS. The LOD and LOQ are 5 and 10 microg/kg, respectively, for these two analytes using GC-ECD. For GC-MS, LOD and LOQ were 2 and 5 microg/kg, respectively. The rapid and reliable method can be used for characterization and quantification of residues of amitraz and its main metabolite, 2,4-dimethylaniline, in liver and kidney samples of swine, sheep and bovine.
authors.affiliation: National Reference Laboratory of Veterinary Drug Residues & MOA Key Laboratory of Food Safety Evaluation, Huazhong Agricultural University, Wuhan 430070, PR China. yh881@163.com
authors.forename: Huan
authors.initials: H
authors.lastname: Yu
authors.forename: Yanfei
authors.initials: Y
authors.lastname: Tao
authors.forename: Tao
authors.initials: T
authors.lastname: Le
authors.forename: Dongmei
authors.initials: D
authors.lastname: Chen
authors.forename: Awais
authors.initials: A
authors.lastname: Ishsan
authors.forename: Yu
authors.initials: Y
authors.lastname: Liu
authors.forename: Yulian
authors.initials: Y
authors.lastname: Wang
authors.forename: Zonghui
authors.initials: Z
authors.lastname: Yuan
mesh_terms: D000814:Aniline Compounds / Q000032:analysis; D000818:Animals; D002417:Cattle; D005504:Food Analysis / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006586:Hexanes / Q000737:chemistry; D007668:Kidney / Q000737:chemistry*; D008099:Liver / Q000737:chemistry*; D000432:Methanol / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012756:Sheep; D052616:Solid Phase Extraction; D013552:Swine; D014052:Toluidines / Q000032:analysis*
chemical_list: D000814:Aniline Compounds; D006586:Hexanes; D014052:Toluidines; C014983:amitraz; C009694:2,4-xylidine; D000432:Methanol