Chinese Journal of Chromatography

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Rapid determination of patulin in apple juice by tert-butyldimethylsilyl derivatization-gas chromatography-mass spectrometry

LI Fengge1*, YAO Weiqin1, TIAN Yanhe1, LI Xuewen2, ZHANG Hongxia2, DOU Hui1, ZHU Huiping1   

  1. 1. Technical Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China; 2. Food Science Institute, Xinjiang Agriculture University, Urumqi 830063, China
  • Received:2010-02-18 Revised:2010-04-18 Online:2010-07-28 Published:1980-03-25
  • Contact: LI Fengge

Abstract: A gas chromatography-mass spectrometry (GC-MS) method for the quantitative determination and confirmation of patulin in apple juice by tert-butyldimethylsilyl (TBDMS) derivatization was established. The sample was extracted with ethyl acetate-hexane and an aliquot of the supernatant was cleaned up using mixed-mode solid phase extraction (SPE) cartridge containing C18 and graphitized carbon black (GCB), evaporated to dryness under nitrogen gas and the residue was converted to tert-butyldimethylsilyl derivative which was determined with GC-MS in selected ion monitoring (SIM) mode and external standard method was used for quantitative determination. The linear range was from 0.01 to 1 mg/L. The average recoveries were 88%~98% and relative standard deviations were 5.3%~13.6% in the spiked range of 2~50 μg/kg. The limit of detection was 0.5 μg/kg and the limit of quantification and confirmation was 2 μg/kg. The method is rapid, highly sensitive, accurate, specific, rugged and suitable for the quantitative determination and confirmation of patulin in apple juice.

Key words: apple juice, patulin , tert-butyldimethylsilyl (TBDMS), gas chromatography-mass spectrometry (GC-MS)