色谱 ›› 2019, Vol. 37 ›› Issue (1): 2-7.DOI: 10.3724/SP.J.1123.2018.09014

• 特别策划:南京海关动植物与食品检测中心专栏 • 上一篇    下一篇

高效液相色谱-串联质谱法测定蔬菜水果中双甲脒及其代谢产物

黄娟, 桂茜雯, 高玲, 张晓燕, 沈伟健, 吴斌, 丁涛   

  1. 南京海关动植物与食品检测中心, 江苏 南京 210019
  • 收稿日期:2018-09-21 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 黄娟,Tel:(025)52345178,E-mail:huang-juan@yeah.net.
  • 基金资助:

    政府间国际科技创新合作重点专项(2017YFE0110800).

Determination of amitraz and its metabolites in vegetables and fruits by high performance liquid chromatography-tandem mass spectrometry

HUANG Juan, GUI Qianwen, GAO Ling, ZHANG Xiaoyan, SHEN Weijian, WU Bin, DING Tao   

  1. Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China
  • Received:2018-09-21 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    Key Project of International Scientific and Technological Innovation Cooperation between Governments (No. 2017YFE0110800).

摘要:

建立了高效液相色谱-串联质谱(HPLC-MS/MS)检测蔬菜水果中双甲脒(AMZ)及其降解或代谢产物单甲脒(DMPF)、2,4-二甲基苯基甲酰胺(DMF)和2,4-二甲基苯胺(DMA)的分析方法。样品经0.1 mol/L NaOH溶液稀释、正己烷-异丙醇(2:1,v/v)混合提取液提取,然后采用HPLC-MS/MS对目标物进行定性确证和定量分析。采用Phenomenex Kinetex C18色谱柱(100 mm×4.6 mm,2.6 μm)分离,以0.1%(v/v)甲酸水溶液和甲醇为流动相进行梯度洗脱,采用电喷雾电离(ESI)源、正离子监测模式进行检测。在1.0~200.0 μg/L范围内,4种目标化合物呈良好的线性关系,相关系数(r)大于0.99;方法的定量限为0.01~0.4 μg/kg。4种目标化合物在0.5、5.0和20.0 μg/kg 3个水平下的加标回收率为62.5%~105.0%,RSD为7.5%~17.6%。该法简便快捷,准确可靠,灵敏度高,定量限满足目前国内外残留限量要求。

关键词: 2, 2, 4-二甲基苯胺, 4-二甲基苯基甲酰胺, 代谢产物, 单甲脒, 高效液相色谱-串联质谱, 蔬菜水果, 双甲脒

Abstract:

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 n-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 (r>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.

Key words: 2,4-dimethylaniline(DMA), 2,4-dimethylformamidine (DMF), amitraz (AMZ), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), metabolites, semiamitraz (DMPF), vegetables and fruits

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