Citation: LI Jianxun, WANG Yuzhen, WU Cuiling, YANG Xia, SHAN Jihao, FAN Bei. Simultaneous Determination of Amitraz and Their Metabolites in Pork and Porcine Liver by Enhanced Matrix Removal-Lipid Column Purified/Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Applied Chemistry, ;2020, 37(8): 969-976. doi: 10.11944/j.issn.1000-0518.2020.08.200134 shu

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 Jianxun ^a ,
WANG Yuzhen ^a ,
WU Cuiling ^b ,
YANG Xia ^c ,
SHAN Jihao ^a,, ,
FAN Bei ^a,,

a.
Key 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
b.
Agilent Technologies(China) Co., Ltd, Beijing 100102, China
c.
Agilent Technologies(Shanghai) Co., Ltd, Shanghai Pudong New Area, Shanghai 200131, China

Corresponding author: SHAN Jihao, shanjihao2007@163.com FAN Bei, fanbei517@163.com
Received Date: 8 May 2020
Revised Date: 2 June 2020
Accepted Date: 9 June 2020

Fund Project: the National Major R & D Program Funding No. 2018YFF0212800the National Major R & D Program Funding(No.2018YFF0212800, No.2018YFF0212801)the National Major R & D Program Funding No.2018YFF0212801

Figures(6)

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 C₁₈ 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.
- pork,
- liver,
- amitraz,
- metabolites,
- liquid chromatography-tandem mass spectrometry,
- solid-phase extraction
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