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Apr 23, 2014 - Dopant-Assisted Atmospheric Pressure Photoionization of Patulin in Apple Juice and Apple-Based Food with Liquid Chromatography–Tandem...
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Dopant-Assisted Atmospheric Pressure Photoionization of Patulin in Apple Juice and Apple-Based Food with Liquid Chromatography− Tandem Mass Spectrometry Kai Zhang,*,† Jon W. Wong,† Huy Mai,‡ and Mary W. Trucksess† †

Center for Food Safety and Applied Nutrition, Office of Regulatory Science, U.S. Food and Drug Administration, HFS-706, 5100 Paint Branch Parkway, College Park, Maryland 20740, United States ‡ Office of Regulatory Affairs, Kansas City District Laboratory, U.S. Food and Drug Administration, 11630 West 80th Street, Lenexa, Kansas 66214, United States S Supporting Information *

ABSTRACT: A dopant-assisted atmospheric pressure photoionization (APPI) with liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed to determine patulin in apple juice and apple-based food. Different dopants, dopant flow rates, and LC separation conditions were evaluated. Using toluene as the dopant, the LC-APPI-MS/MS method achieved a linear calibration from 12.5 to 2000 μg/L (r2 > 0.99). Matrix-dependent limits of quantitation (LOQs) were from 8 μg/L (solvent) to 12 μg/L (apple juice). [13C]-Patulin-fortified apple juice samples were directly analyzed by the LC-APPI-MS/ MS method. Other apple-based food was fortified with [13C]-patulin, diluted using water (1% formic acid), centrifuged, and filtered, followed by LC-APPI-MS/MS analysis. In clear apple juice, unfiltered apple cider, applesauce, and apple-based baby food, average recoveries were 101 ± 6% (50 μg/kg), 103 ± 5% (250 μg/kg), and 102 ± 5% (1000 μg/kg) (av ± SD, n = 16). Using the suggested method, patulin was detected in 3 of 30 collected market samples with concentrations ranging from