FOOD SCIENCE ›› 2014, Vol. 35 ›› Issue (4): 111-115.doi: 10.7506/spkx1002-6630-201404023

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Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry Combined with QuEChERS for the Quick Detection of Fenbutatin Oxide Residue in Citrus

ZHU Yan-mei1,2, ZHAO Qi-yang1, CHEN Wei-jun1, JIAO Bi-ning1,2,3,*, ZHANG Yao-hai1   

  1. 1. Laboratory of Quality and Safety Risk Assessment for Citrus Products (Chongqing), Ministry of Agriculture, Citrus Research
    Institute, Southwest University, Chongqing 400712, China; 2. College of Food Science, Southwest University,
    Chongqing 400715, China; 3. National Citrus Engineering Research Center, Citrus Research Institute, Chinese Academy of
    Agricultural Sciences, Chongqing 400712, China
  • Received:2013-05-01 Revised:2014-01-06 Online:2014-02-25 Published:2014-03-17
  • Contact: Bining Jiao E-mail:bljiao@tom.com

Abstract:

The fenbutatin oxide residue in citrus fruits was detected by optimized QuEChERS combined with ultraperformance
liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). Fenbutatin oxide was extracted from the
samples with acetonitrile, salted out with anhydrous MgSO4 and NaCl, cleaned up with octadecyl bonded phase silica gel
and then analyzed by UPLC-MS-MS in multiple reaction monitoring (MRM) mode. The separation of the target pesticide
residue was performed on an BEH C18 column (2.1 mm×50 mm) using a mobile phase consisting of 0.1% formic acidmethanol
by isocratic elution and the matrix-matched external standard calibration was used for quantitation. There was a
linear relation between fenbutatin oxide content and peak area in the range of 0.001–1.0 mg/L (R2 ≥ 0.993 0), and the limit
of quantitation was 2.0 μg/kg. The average recoveries in different matrices (citrus pulp, peel and whole fruits) at three spiked
concentration levels ranged from 74.0% to 97.7% with relative standard deviations (RSDs) of 2.5%–6.9%. This method was
simple, quick, cheap, environmentally friendly and safe. The accuracy and precision could meet the requirements for quick
confirmation and quantitative determination of trace fenbutatin oxide residue in citrus fruits.

Key words: QuEChERS, ultra-performance liquid chromatography-tandem mass spectrometry, citrus, fenbutatin oxide

CLC Number: