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

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 microg/kg. The limit of detection was 0.5 microg/kg and the limit of quantification and confirmation was 2 microg/kg. The method is rapid, highly sensitive, accurate, specific, rugged and suitable for the quantitative determination and confirmation of patulin in apple juice.