ABSTRACT
A simultaneous analytical method was developed for the determination of alkyl furans (Furan, 2-methylfuran, 3-methylfuran and 2,5-dimethylfuran) in processed foods by headspace-GC-MS. Single-laboratory validation data of furan, 2-methylfuran, 3-methylfuran and 2,5-dimethylfuran showed good precision and accuracy. The mean recoveries ranged from 92 to 116%, the intermediate precision (RSDi) ranged from 0.9 to 12.9%. The level of LOQ ranged from 0.5 to 1.2 µg/kg (coffee), from 3.5 to 4.1 µg/kg (soy sauce), from 0.4 to 1.3 µg/kg (other foods: clear apple juice, infant formula and baby food), respectively. This method has the sensitivity to detect low levels of furan and alkyl furans contaminated in various foods and is thus applicable to surveillance for risk management in food safety.
Subject(s)
Food, Processed , Furans , Infant , Humans , Coffee , Food SafetyABSTRACT
BACKGROUND: In Japan, the residue definition for fosetyl-Al is "sum of fosetyl-Al and phosphonic acid expressed as fosetyl-Al" and its current provisional maximum residue limit (MRL) in cereals is under review. OBJECTIVE: For establishment and enforcement of fosetyl-Al MRL in cereals, a new analytical method for fosetyl-Al and phosphonic acid in cereals should be developed and validated. METHOD: The new method involves water extraction, cleanup using tandem cation- and anion-exchange mini columns, and determination by LC-MS/MS. It was validated in a single laboratory and multiple laboratories. Using the method, 41 samples of rice, wheat, and barley were analyzed. RESULTS: In the multiple-laboratory validation: repeatability and reproducibility for three concentrations of fosetyl-Al and phosphonic acid were in ranges of 4.8-20 and 5.9-34%; calculated sum of fosetyl-Al and phosphonic acid, expressed as fosetyl-Al, showed good recoveries; linearity was observed for fosetyl-Al and phosphonic acid in ranges of 0.005-0.4 and 0.025-2.0 mg/kg; and specificity was sufficient. The method was verified for rice matrixes. In 41 samples, phosphonic acid was detected up to 0.2 mg/kg while fosetyl was not. CONCLUSIONS: The method was successfully validated with high precision, accuracy, linearity, and specificity and capable of analyzing fosetyl-Al and phosphonic acid with a practical LOQ of 0.01 and 0.05 mg/kg. The LOQs and concentrations of phosphonic acid in samples indicate that a potential MRL would be 0.5 mg/kg for fosetyl-Al in cereals. HIGHLIGHTS: The validated method was simpler than many methods and did not require derivatization, matrix-matched orisotopically-labeled internal standards.
