Rapid gas chromatography/mass spectrometry determination and confirmation of patulin in apple juice
1U.S. Food and Drug Administration, Pacific Regional Laboratory Northwest, Bothell, WA 98021, USA. heidi.marks@fda.hhs.gov
Abstract:
A gas chromatography/mass spectrometry (GC/MS) method was developed for the quantitative determination and confirmation of patulin extracted from apple juice. Juice is alkalized and extracted with ethyl acetate-hexane, a portion concentrated under N2, then resolubilized in acetonitrile for simple derivatization with bis(trimethylsilyl)trifluoracetamide. Patulin was determined by GC/MS using an electron-impact source and selected ion monitoring of characteristic ions. Spike levels of 20-100 microg/L gave an average recovery of 86%, and 6 ions of sample and standard spectra matched within 10% absolute for confirmation. The limits of quantitation and detection were 10 and 3 microg/L, respectively.
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