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Determination of Diclazuril in Fish by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

XING Lihong, SUN Weihong*, SUN Xiaojie, LI Zhaoxin, GUO Jiangtao   

  1. Yellow Sea Fisheries Research Institute, Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality,
    Ministry of Agriculture, Laboratory of Quality and Safety Risk Assessment for Aquatic Products (Qingdao), Ministry of Agriculture,
    Chinese Academy of Fishery Sciences, Qingdao 266071, China
  • Online:2016-07-25 Published:2016-07-26
  • Contact: SUN Weihong

Abstract:

A method has been developed for the determination of diclazuril in fish by high performance liquid
chromatography-tandem mass spectrometry (HPLC-MS/MS) with dispersive solid phase extraction. Samples were
dehydrated with anhydrous sodium sulfate, and extracted with acetonitrile. Then the extracts were concentrated under
vacuum condition. The samples were degreased with hexane and cleaned up by dispersive solid phase extraction, analyzed
by HPLC-MS/MS and quantified with internal standard method. Electrospray ionization was applied and operated in the
negative ion mode. The calibration curve showed good linearity between peak area and the concentration of diclazuril
in the range of 1–100 μg/L with a correlation coefficient over 0.999. The average recoveries from spiked sample at the
three concentrations of 1.00, 5.00 and 50.0 μg/kg ranged from 95.4% to 108% with intra- and inter-batch relative standard
deviations below 15%. The limit of detection (LOD) for diclazuril was 0.50 μg/kg. This efficient and simple method could
be used to identify and quantify diclazuril in fish with satisfactory sensitivity and repeatability.

Key words: dispersive solid phase extraction, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), fish, diclazuril

CLC Number: