Chinese Journal of Applied Chemistry ›› 2020, Vol. 37 ›› Issue (8): 969-976.DOI: 10.11944/j.issn.1000-0518.2020.08.200134

• Full Papers • Previous Articles    

Simultaneous Determination of Amitraz and Their Metabolites in Pork and Porcine Liver by Enhanced Matrix Removal-Lipid Column Purified/Liquid Chromatography-Tandem Mass Spectrometry

LI Jianxuna, WANG Yuzhena, WU Cuilingb, YANG Xiac, SHAN Jihaoa*, FAN Beia*   

  1. aKey Laboratory of Agricultural Product Quality and Safety Collection,Storage,Transportation, and Control of the Ministry of Agriculture and Rural Affairs,Institute of Agricultural Products Processing,Chinese Academy of Agricultural Sciences,Beijing 100193,China;
    bAgilent Technologies (China) Co.,Ltd,Beijing 100102,China;
    cAgilent Technologies(Shanghai) Co.,Ltd,Shanghai Pudong New Area,Shanghai 200131,China
  • Received:2020-05-08 Online:2020-08-01 Published:2020-08-07
  • Contact: SHAN Jihao, senior engineer; Tel/Fax:010-62817417;; Research interests:veterinary drug residue detection; FAN Bei, professor; Tel/Fax:010-62817417;; Research interests:agricultural product quality and safety risk assessment
  • Supported by:
    National Major R & D Program Funding(No.2018YFF0212800, No.2018YFF0212801)

Abstract: An analytical method based on enhanced matrix removal(EMR)-Lipid column purified/liquid chromatography-tandem mass spectrometry was developed for the determination of amitraz (AMZ) and their metabolites 2,4-xylidine (DMA), semiamitraz (DMPF) and N-(2,4-dimethylphenyl)formamide (DMF) residues in pork and porcine liver. The pork and porcine liver samples were precipitated with acetonitrile and salting out with extraction. The acetonitrile supernatant was cleaned up with Captiva EMR-Lipid cartridge, and then the supernatant solution was filtered through a nylon membrane into a glass LC sample vial for LC-MS/MS analysis. The solution was separated on an Agilent ZORBAX Eclipse Plus column (50 mm×2.1mm, 1.8 μm) with 0.1% formic acid acetonitrile-0.1% formic acid solution as mobile phases by gradient elution, then determined by LC-MS/MS with electrospray ionization (ESI) in positive ion scanning mode under multiple reaction monitoring (MRM) mode. The results show that the linear range of AMZ, DMA in pig liver and pork is 1~200 μg/kg, while the linear range of DMPF and DMF is 0.1~200 μg/kg, The correlation coefficient (R2) is greater than 0.991; The quantitative limits of AMZ, DMA, DMPF and DMF are 0.6, 0.6, 0.05, 0.05 μg/kg, respectively; The spiked recoveries at four levels of 0.1, 1, 5, and 50 μg/kg are in the range of 60.2%~127.4% with relative standard deviations (RSD) lower than 12%. This method provides an easy and fast detection technique for the analysis of AMZ and its metabolites residues in pork and porcine liver samples.

Key words: pork, liver, amitraz, metabolites, liquid chromatography-tandem mass spectrometry, solid-phase extraction