Development and Validation of Methodology for Determination of Furfuryl Alcohol in Snack Foods and Their Ingredients by Headspace Gas Chromatography-Mass Spectrometry

A static headspace gas chromatography-mass spectrometry (HS-GC-MS) method was developed for determination of furfuryl alcohol (FFA) in snack foods and related ingredients, achieving low limits of detection and quantification (LOQs) in a wide range of matrices. The method employs extraction of samples (5 g) with deionized water (25 mL), followed by the HS-GC-MS analysis of the extract. This approach provides more consistent results for a wide range of matrix types when compared to in-vial sample extraction HS-GC-MS. Stable isotopically labeled internal standard (FFA-D-5) is added to the samples prior to the extraction. Method validation studies were conducted over multiple days in representative matrices, which were selected based on their carbohydrate, protein, and fat content (categories 2, 5, and 6 of the AOAC food matrix triangle). Acceptable linearity was obtained with correlation coefficients higher than 0.995. The optimized method delivered a LOQ of 0.5 mg/kg or less in a variety of snack foods. Average fortification recoveries were within 80-120% with inter-day relative standard deviation below 20%. The results indicated acceptable accuracy and ruggedness of the methodology for routine determination of FFA in a variety of snack foods.