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Simultaneous Determination of Four Mycotoxins in Citrus Fruits by Ultra Performance Liquid Chromatography- Electrospray Ionization Tandem Mass Spectrometry Combined with Modified QuEChERS

SHI Wen-jing1,2, ZHAO Qi-yang1, JIAO Bi-ning1,2,3,*   

  1. 1. Laboratory of Quality and Safety Risk Assessment for Citrus Products, Ministry of Agriculture, Citrus Research Institute,
    Southwest University, Chongqing 400712, China; 2. College of Horticulture and Landscape Architecture, Southwest University,
    Chongqing 400715, China; 3. National Citrus Engineering Research Center, Citrus Research Institute,
    Chinese Academy of Agricultural Sciences, Chongqing 400712, China
  • Online:2014-10-25 Published:2014-11-07

Abstract:

A method was developed for simultaneous determination of four mycotoxins (aletrnariol monomethyl ether,
tentoxin, alternariol, and citrinin) in citrus fruits using ultra-performance liquid chromatography-tandem mass spectrometry
combined with optimized QuEChERS. Samples were extracted with acetonitrile, salted out with anhydrous MgSO4 and
NaCl, cleaned up with C18 and then analyzed using UPLC-MS-MS in multiple reaction monitoring (MRM) mode with
electrospray ionization. The separation of the target mycotoxins was performed on an ACQUITY UPLC BEH C18 liquid
chromatography column through gradient elution using a mobile phase consisting of acetonitrile and 0.1% formic acid
aqueous solution and the matrix-matched external standard calibration was used for quantitation. This method had a good
linearity in the concentration range of 5.0–200 μg/L with correlation coefficients (R2) more than 0.992 7, and the limit of
detection of the established method was in the range of 0.2–0.7 μg/kg. The average recoveries of the four mycotoxins in
different matrixes (citrus pulp, peel and whole fruit) at three spiked levels ranged from 78.0% to 103.3%, with relative
standard deviations (RSDs) of 2.6%–10.6%. This method is simple, quick, accurate, sensitive, and suitable for the quick
confirmation and quantitative determination of the four mycotoxins in citrus fruits.

Key words: ultra-high liquid chromatography-electrospray ionization tandem mass spectrometry, QuEChERS, citrus, mycotoxins

CLC Number: