Huang Juan, Gui Qianwen, Gao Ling, Zhang Xiaoyan, Shen Weijian, Wu Bin, Ding Tao
Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China.
Se Pu. 2019 Jan 8;37(1):2-7. doi: 10.3724/SP.J.1123.2018.09014.
A method was established for the determination of amitraz (AMZ), and its metabolites semiamitraz (DMPF), 2,4-dimethylformamidine (DMF) and 2,4-dimethylaniline (DMA) in vegetables and fruits by using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were diluted with 0.1 mol/L sodium hydroxide and extracted with -hexane-isopropanol (2:1, v/v). The separation was performed on a Phenomenex Kinetex C18 column (100 mm×4.6 mm, 2.6 μm) with gradient elution using 0.1% (v/v) formic acid aqueous solution-methanol as the mobile phase. The analysis of amitraz and its metabolites were detected under electrospray positive ionization mode. The limits of quantification (LOQs) were between 0.01 and 0.4 μg/kg. The good linearities (>0.99) were achieved for the target compounds in the range of 1.0-200.0 μg/L. The recoveries at three spiked levels (0.5, 5.0 and 20 μg/kg) in blank matrix were in the range of 62.5%-105.0% with the relative standard deviations between 7.5% and 17.6%. The method is convenient, rapid, accurate, efficient, sensitive and practical. It is suitable for the determination and confirmation of amitraz and its metabolites in vegetables and fruits, and can meet the demands of domestic and foreign regulations.
建立了一种利用高效液相色谱 - 串联质谱法（HPLC - MS/MS）测定蔬菜和水果中双甲脒（AMZ）及其代谢产物二甲双甲脒（DMPF）、2,4 - 二甲基甲脒（DMF）和2,4 - 二甲基苯胺（DMA）的方法。样品用0.1 mol/L氢氧化钠稀释，并用正己烷 - 异丙醇（2:1，v/v）萃取。在Phenomenex Kinetex C18柱（100 mm×4.6 mm，2.6 μm）上进行分离，以0.1%（v/v）甲酸水溶液 - 甲醇为流动相进行梯度洗脱。双甲脒及其代谢产物的分析在电喷雾正离子化模式下进行检测。定量限（LOQs）在0.01至0.4 μg/kg之间。目标化合物在1.0 - 200.0 μg/L范围内具有良好的线性关系（>0.99）。在空白基质中三个加标水平（0.5、5.0和20 μg/kg）下的回收率在62.5% - 105.0%之间，相对标准偏差在7.5% - 17.6%之间。该方法简便、快速、准确、高效、灵敏且实用。适用于蔬菜和水果中双甲脒及其代谢产物的测定和确证，能够满足国内外法规要求。
