Validation of the Analytical Procedure for the Determination of Malondialdehyde and Three Other Aldehydes in Vegetable O
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Validation of the Analytical Procedure for the Determination of Malondialdehyde and Three Other Aldehydes in Vegetable Oil Using Liquid Chromatography Coupled to Tandem Mass Spectrometry (LC-MS/MS) and Application to Linseed Oil Caroline Douny & Angélique Tihon & Pierre Bayonnet & François Brose & Guy Degand & Eric Rozet & Jérôme Milet & Laurence Ribonnet & Loranne Lambin & Yvan Larondelle & Marie-Louise Scippo
Received: 8 July 2014 / Accepted: 23 October 2014 # Springer Science+Business Media New York 2014
Abstract Secondary oxidation products of fatty acids, mainly aldehydes, are susceptible to cause significant deterioration in chemical, sensory and nutritional food properties, as well as adverse health effects. An analytical method involving separation by liquid chromatography coupled to the detection by tandem mass spectrometry (LC-MS/MS) has been developed to evaluate the concentration of four aldehydes in oil samples: malondialdehyde (MDA), 4-hydroxy-2-nonenal (4-HNE), 4hydroxy-2-hexenal (4-HHE) and 2,4-decadienal (2,4-DECA). The optimisation of the extraction, derivation, detection and quantification has been finalised for coconut oil, used as a model of vegetable oils. The method has been validated according to the criteria and procedure described in international standards. The evaluated parameters include specificity/ selectivity, recovery, precision, accuracy, uncertainty, limits of detection and quantification, using the concept of accuracy profiles. These parameters have been evaluated during experiments planned on different non-consecutive days with coconut oil spiked at different levels of concentration. The C. Douny (*) : A. Tihon : P. Bayonnet : F. Brose : G. Degand : M.159
6.0
30
+
235>189 249>173
6.0
32
4-HHE-DNPH
−
249>203 293>163
5.0
29
4-HNE-DNPH
−
293>167 335>167
4.0
32
−
335>288 331>230
1.5
34
MeMDA-DNPH
2,4-decadienal-DNPH
331>284
Germany), according to the Schaal oven test. Temperature in oven was monitored during the test with temperature probe from VWR International (Radnor, Pennsylvania), with a measurement uncertainty of 0.5 °C. After 0, 3, 4, 6, 12 and 24 days, bottles were removed from the oven, flushed with nitrogen, closed and stored at −80 °C until analysis. Samples were analysed in triplicate on three independent experiments, with three different batches of 1PLO, leading to nine samples per day of storage and a total of 54 samples.
tested using the analysis of the variance and generalised linear models (GLM) procedure of JMP® software. Levels of significant effects were compared using least square means and associated standard error (significant for P
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