Rapid gas chromatography/mass spectrometry determination and confirmation of patulin in apple juice. 2007

Heidi S Marks
U.S. Food and Drug Administration, Pacific Regional Laboratory Northwest, Bothell, WA 98021, USA. heidi.marks@fda.hhs.gov

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.

UI MeSH Term Description Entries
D007477 Ions An atom or group of atoms that have a positive or negative electric charge due to a gain (negative charge) or loss (positive charge) of one or more electrons. Atoms with a positive charge are known as CATIONS; those with a negative charge are ANIONS.
D008401 Gas Chromatography-Mass Spectrometry A microanalytical technique combining mass spectrometry and gas chromatography for the qualitative as well as quantitative determinations of compounds. Chromatography, Gas-Liquid-Mass Spectrometry,Chromatography, Gas-Mass Spectrometry,GCMS,Spectrometry, Mass-Gas Chromatography,Spectrum Analysis, Mass-Gas Chromatography,Gas-Liquid Chromatography-Mass Spectrometry,Mass Spectrometry-Gas Chromatography,Chromatography, Gas Liquid Mass Spectrometry,Chromatography, Gas Mass Spectrometry,Chromatography, Mass Spectrometry-Gas,Chromatography-Mass Spectrometry, Gas,Chromatography-Mass Spectrometry, Gas-Liquid,Gas Chromatography Mass Spectrometry,Gas Liquid Chromatography Mass Spectrometry,Mass Spectrometry Gas Chromatography,Spectrometries, Mass-Gas Chromatography,Spectrometry, Gas Chromatography-Mass,Spectrometry, Gas-Liquid Chromatography-Mass,Spectrometry, Mass Gas Chromatography,Spectrometry-Gas Chromatography, Mass,Spectrum Analysis, Mass Gas Chromatography
D009183 Mycotoxins Toxic compounds produced by FUNGI. Fungal Toxins,Mycotoxin,Toxins, Fungal
D010365 Patulin 4-Hydroxy-4H-furo(3,2-c)pyran-2(6H)-one. A mycotoxin produced by several species of Aspergillus and Penicillium. It is found in unfermented apple and grape juice and field crops. It has antibiotic properties and has been shown to be carcinogenic and mutagenic and causes chromosome damage in biological systems.
D002138 Calibration Determination, by measurement or comparison with a standard, of the correct value of each scale reading on a meter or other measuring instrument; or determination of the settings of a control device that correspond to particular values of voltage, current, frequency or other output. Calibrations
D002623 Chemistry Techniques, Analytical Methodologies used for the isolation, identification, detection, and quantitation of chemical substances. Analytical Chemistry Techniques,Analytical Chemistry Methods,Analytical Chemistry Method,Analytical Chemistry Technique,Chemistry Method, Analytical,Chemistry Methods, Analytical,Chemistry Technique, Analytical,Method, Analytical Chemistry,Methods, Analytical Chemistry,Technique, Analytical Chemistry,Techniques, Analytical Chemistry
D005504 Food Analysis Measurement and evaluation of the components of substances to be taken as FOOD. Analysis, Food,Analyses, Food,Food Analyses
D005506 Food Contamination The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage. Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D001628 Beverages Liquids that are suitable for drinking. (From Merriam Webster Collegiate Dictionary, 10th ed) Beverage
D013058 Mass Spectrometry An analytical method used in determining the identity of a chemical based on its mass using mass analyzers/mass spectrometers. Mass Spectroscopy,Spectrometry, Mass,Spectroscopy, Mass,Spectrum Analysis, Mass,Analysis, Mass Spectrum,Mass Spectrum Analysis,Analyses, Mass Spectrum,Mass Spectrum Analyses,Spectrum Analyses, Mass

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