The ability of the spectrophotometric thiobarbituric acid reactive substances (TBARS) test to determine malondialdehyde (MDA) in various food matrices was evaluated. MDA was extracted from the foods; the extract reacted with thiobarbituric acid (TBA); and the formed TBA-MDA adduct was measured spectrophotometricaly at 532 nm. In parallel, the TBA-MDA adduct was analyzed with high-performance liquid chromatography (HPLC) coupled with fluorescence detection. Oils and unprocessed and uncooked meat and fish products did not exhibit any significant difference in the amount of MDA measured by the two methods, indicating that the major substance reacting with TBA and forming an adduct that absorbs at 532 nm was MDA. However, in products such as dry nuts, pork sausages, cooked fish, and gouda cheese, an overestimation of MDA was observed, indicating that TBARS test was unsuitable for accurate determination of MDA. Furthermore, the results in the present work suggest that the overestimation of MDA by the TBARS test as it was applied is related to the interference of other than secondary lipid oxidation products.
A reliable and suitable method for the determination of epoxy fatty acids in various food matrices based on the Bligh and Dyer lipid extraction procedure was developed and validated. The method involves the use of a methylated epoxy fatty acid as internal standard (IS), extraction of the analytes from the matrices followed by room temperature methylation, a three-step solid phase extraction (SPE) separation of the fatty acid methyl esters (FAMEs), and detection with gas chromatography-flame ionization detection (GC-FID). The method was validated in four different food matrices chosen as model systems, namely, vegetable oils, unprocessed pork, fried potato crisps, and infant formula. The extraction technique allows the method to be applied for routine analysis of a large amount of samples. Intraday repeatability ranged from 1 to 19%, and interday reproducibility ranged from 2 to 9%. The limit of quantification (LOQ) ranged from 3.32 to 20.47 μg g(-1) of sample with recoveries ranging from 94 to 115%. The results verify the accuracy and reproducibility of the analytical technique and its ability to provide reliable quantification of epoxy fatty acids. Finally, levels of epoxy fatty acids in several food products on the Belgian market were screened and are presented.
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