National Reference Laboratory of Veterinary Drug Residues & MOA Key Laboratory of Food Safety Evaluation, Huazhong Agricultural University, Wuhan 430070, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Jul 1;878(21):1746-52. doi: 10.1016/j.jchromb.2010.04.034. Epub 2010 Apr 29.
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.
一种新的方法已经发展到决心和确认的脒和其主要代谢物，2,4-二甲基苯胺，在食品动物组织中使用气相色谱 - 电子捕获检测器（GC-ECD）和气相色谱 - 质谱检测器（GC-MS）。该方法是基于一个新的提取程序使用加速溶剂萃取（ASE）。它包括一个正己烷/甲醇提取步骤，清洁了一步贝克邦德十八烷基 C（18）硅胶键合柱，水解和衍生为 2,4-二甲基-7-F-丁酰胺 GC-ECD 分析。为了确认使用 GC-MS，水解和衍生是不需要的。萃取压力、温度和循环参数的 ASE、清洁、衍生和分析程序已经得到了优化。从 50 到 300 微克/公斤的水平的刺回收率发现之间 72.4 和 101.3%与相对标准偏差小于 11.5%在 GC-ECD，从 5 到 20 微克/公斤的水平发现之间 77.4 和 107.1%与相对标准偏差小于 11.6%在 GC-MS。LOD 和 LOQ 分别为 5 和 10 微克/公斤，这两种分析物使用 GC-ECD。GC-MS 的 LOD 和 LOQ 分别为 2 和 5 微克/公斤。快速、可靠的方法可以用来描述和量化残留的脒和其主要代谢物，2,4-二甲基苯胺，在肝和肾组织的猪、羊和牛。
