Static Headspace Gas Chromatographic Method for Aldehyde Determination in Crackers

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Static Headspace Gas Chromatographic Method for Aldehyde Determination in Crackers Anamarija I. Mandić & Ivana J. Sedej & Marijana B. Sakač & Aleksandra Č. Mišan

Received: 27 January 2012 / Accepted: 3 April 2012 / Published online: 25 April 2012 # Springer Science+Business Media, LLC 2012

Abstract The aim of this work was to develop and validate static headspace gas chromatography with flame ionization detection method for determination of five aldehydes selected as markers for lipid oxidation, present in freshly baked and stored crackers with high fat content. Chromatographic conditions defined in this method allow the separation of propanal, pentanal, hexanal, heptanal and octanal within 15 min. Relative standard deviations (RSD) of the retention times for repeatability and intermediate precision for all compounds were less than 1.75 and 0.22 %, respectively. For the obtained peak areas, RSD for repeatability and intermediate precision were less than 3.86 and 4.32 %, respectively. Recovery was within the range of 60–99 %. Each analyte showed an excellent linear behaviour over the set concentration range, with correlation coefficient (R2) values above 0.99. Limits of quantification for propanal, pentanal, hexanal, heptanal and octanal were 0.10, 0.05, 0.08, 0.02 and 0.02 μg, respectively. The proposed method accomplishes the requirements for the method selectivity, precision, sensitivity, accuracy and linearity needed for determination of aldehydes in bakery products. Quantification of aldehydes was achieved for both freshly baked and stored crackers over a long period of time. Keywords SHS gas chromatography . Lipid oxidation . Aldehydes . Crackers . Method validation

A. I. Mandić (*) : I. J. Sedej : M. B. Sakač : A. Č. Mišan Institute of Food Technology in Novi Sad, University of Novi Sad, Bulevar cara Lazara 1, 21000 Novi Sad, Serbia e-mail: [email protected]

Introduction Lipid oxidation occurs during processing, storage and handling of lipid containing food and causes its quality deterioration. Reactions of lipid oxidation lead to the formation of a large number of decomposition products. Lipid hydroperoxides, as primary products of lipid oxidation, are unstable and rapidly decompose, yielding a range of secondary lipid oxidation products. Large number of methods have been proposed for measuring the primary and secondary lipid oxidation products, which are based on the evaluation of a single compound or classes of compounds, chosen as markers. Methods for assessing the oxidative damage of lipids in plants, food and in biological systems are thoroughly reviewed in the literature (Watson 2006; Wood et al. 2006; Laguerre et al. 2007; Schneider et al. 2008; Moon and Shibamoto 2009). Off-flavours in food occurr mainly as a result of the formation of volatile compounds, representing a small proportion of the formed lipid oxidation products. Some of them, such as aldehydes, are highly specific to the oxidative degradation of a particular polyunsaturated fatty acids (Laguerre et al. 2007). Gas chromat