Volume 15 Issue 3
Jun.  2019
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JIANG Yongyuan, WANG Qiang, LI Laihao, WANG Xufeng, ZHAO Donghao, CAI Nan, GUAN Wanqi. Determination of quinoxalines and their major metabolites residues in fishmeal by ultra-performance liquid chromatography tandem mass spectrometry[J]. South China Fisheries Science, 2019, 15(3): 14-21. DOI: 10.12131/20180278
Citation: JIANG Yongyuan, WANG Qiang, LI Laihao, WANG Xufeng, ZHAO Donghao, CAI Nan, GUAN Wanqi. Determination of quinoxalines and their major metabolites residues in fishmeal by ultra-performance liquid chromatography tandem mass spectrometry[J]. South China Fisheries Science, 2019, 15(3): 14-21. DOI: 10.12131/20180278
shu

Determination of quinoxalines and their major metabolites residues in fishmeal by ultra-performance liquid chromatography tandem mass spectrometry

  • 1.

    Zhejiang Ocean University, Zhoushan 316021, China

  • 2.

    Key Laboratory of Aquatic Product Processing, Ministry of Agriculture and Rural Affairs; South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Guangzhou 510300, China

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  • Received Date: December 12, 2018
  • Revised Date: January 13, 2019
  • Accepted Date: January 27, 2019
  • Available Online: February 17, 2019
    Graphical Abstract
    • Abstract

  • A sensitive and reliable ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) method was eatablished for the determination of olaquindox (OLA), carbadox (CBX), cyadox (CYA), quinocetone (QCT), mequindox (MEQ) and their main metabolites (QCA and MQCA) in fishmeal. The samples were extracted by acetonitrile-ethyl acetate mixture (1∶1, V∶V) and hydrochloric acid solution (1 mol·L–1), then the analyte which dissolved in the aqueous phase was re-extracted by ethyl acetate. The extraction was concentrated and reconstituted with acetonitrile. After purification with the Oasis PRiME HLB SPE cartridge, the sample was subjected to the following analytical procedure. The mobile phase containing acetonitrile and 0.1% formic acid solution with a linear gradient elution was utilized to separate all compounds on a Phenomenex Kinetex C18 column. The quantitative analysis of metabolites was carried out with an internal standard method and the others with an external standard method in the multiple reaction monitoring mode using positive electrospray ionization. The calibration curves for all compounds were linear (R≥0.994) within their corresponding concentration range. The recoveries were 64.4%−102.2% at different spiking levels with RSDs of 3.2%−10.2%. The limits of detection and quantification of MQCA and QCA were 2 μg·kg–1and 5 μg·kg–1; MEQ was 10 μg·kg–1 and 20 μg·kg–1; the others were 1 μg·kg–1 and 2 μg·kg–1, respectively. This method with high sensitivity and good precision can be applied to the simultaneous determination of quinoxaline drugs and their major metabolite in fishmeal samples.

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