Electron spin resonance (microESR) to determine the peroxide value of virgin olive oil

Authors

DOI:

https://doi.org/10.3989/gya.0759241.2201

Keywords:

electron spin resonance, free radicals, oxidation, peroxide value, virgin olive oil

Abstract


The present study aims to find correlation models between peroxide values (PVs), as determined according to the EU official method, and electron spin resonance (ESR) spectroscopy assay data, in order to use this method as an automated and solventefficient screening tool to assess the oxidative status of virgin olive oils (VOOs). The concentration of free radicals, measured at two times of a specific ESR procedure, and PVs were utilized to create linear regression models. To test them, the PVs of 7 VOO samples (3 VOOs for internal and 4 VOOs for external validation) were determined and, on the same oils, the ESR assay was performed. The results were interpolated in two models, and the PVs predicted by ESR were compared to those obtained using the official method. The two methods showed statistical consistency (p ≤ 0.05). These preliminary findings suggest that the ESR assay is an effective and sustainable screening tool for monitoring the primary oxidative state of VOOs.

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References

Altunkaya A, Hedegaard RV, Harholt J, Brimer L, Gökmen V, Skibsted LH. 2013. Oxidative stability and chemical safety of mayonnaise enriched with grape seed extract. Food Funct. 4 (11), 1647-1653. https://doi.org/10.1039/c3fo60204d PMid:24064585

Bajoub A, Bendini A, Fernández-Gutiérrez A, Carrasco-Pancorbo A. 2018. Olive oil authentication: A comparative analysis of regulatory frameworks with especial emphasis on quality and authenticity indices, and recent analytical techniques developed for their assessment. A review. Crit. Rev. Food Sci. Nutr. 58 (5), 832-857. https://doi.org/10.1080/10408398.2016.1225666 PMid:27657556

Chen H, Cao P, Li B, Sun D, Li J, Liu Y. 2017a. High sensitive and efficient detection of edible oils adulterated with used frying oil by electron spin resonance. Food Control 73, 540-545. https://doi.org/10.1016/j.foodcont.2016.08.050

Chen H, Wang Y, Cao P, Liu Y. 2017b. Effect of temperature on thermal oxidation of palmitic acid studied by combination of EPR spin trapping technique and SPME-GC-MS/MS. Food Chem. 234, 439-444. https://doi.org/10.1016/j.foodchem.2017.04.135 PMid:28551258

Chen Q, Xie Y, Xi J, Guo Y, Qian HE, Cheng Y, Chen Y, Yao W. 2018. Characterization of lipid oxidation process of beef during repeated freeze-thaw by electron spin resonance technology and Raman spectroscopy. Food Chem. 243, 58-64. https://doi.org/10.1016/j.foodchem.2017.09.115 PMid:29146370

Commission Implementing Regulation (EU) 2022/2105 of 29 July 2022 laying down rules on conformity checks of marketing standards for olive oil and methods of analysis of the characteristics of olive oil (accessed on 10 July 2024).

Commission Delegated Regulation (EU) 2022/2104 of 29 July 2022 supplementing Regulation (EU) No 1308/2013 of the European Parliament and of the Council as regards marketing standards for olive oil, and repealing Commission Regulation (EEC) No 2568/91 and Commission Implementing Regulation (EU) No 29/2012 (accessed on 10 July 2024).

Conte L, Bendini A, Valli E, Lucci P, Moret S, Maquet A, Lacoste F, Brereton P, García-González DL, Moreda W, Gallina Toschi T. 2019. Olive oil quality and authenticity: A review of current EU legislation, standards, relevant methods of analyses, their drawbacks and recommendations for the future. Trends Food Sci. Technol. 105, 483-493. https://doi.org/10.1016/j.tifs.2019.02.025

Cui L, Lahti PM, Decker EA. 2017. Evaluating electron paramagnetic resonance (EPR) to measure lipid oxidation lag phase for shelf-life determination of oils. J. Am. Oil Chem.Soc. 94 (1), 89-97. https://doi.org/10.1007/s11746-016-2927-1

Cui N, Wang G, Ma Q, Zhao T, Han Z, Yang Z, Liang L. 2021. Evolution of lipid characteristics and minor compounds in hazelnut oil based on partial least squares regression during accelerated oxidation process. LWT 150, 112025. https://doi.org/10.1016/j.lwt.2021.112025

Fadda A, Montoro P, D'Urso G, Ravasio, N Zaccheria F, Sanna D. (2023). Sustainable Extraction Methods Affect Metabolomics and Oxidative Stability of Myrtle Seed Oils Obtained from Myrtle Liqueur By-Products: An Electron Paramagnetic Resonance and Mass Spectrometry Approach. Antioxidants 12 (1), 154. https://doi.org/10.3390/antiox12010154 PMid:36671016 PMCid:PMC9854790

Frankel EN. 2010. Chemistry of extra virgin olive oil: adulteration, oxidative stability, and antioxidants. J. Agric. Food Chem. 58 (10), 5991-6006. https://doi.org/10.1021/jf1007677 PMid:20433198

Frankel EN. 1980. Lipid oxidation, in Progress in Lipid Research, 19 (1-2), 1-22. https://doi.org/10.1016/0163-7827(80)90006-5 PMid:7232452

Frankel EN. 1983. Volatile lipid oxidation products, in Progress in Lipid Research 22 (1), 1-33. https://doi.org/10.1016/0163-7827(83)90002-4 PMid:6306693

Frega N, Mozzon M, Lercker G. 1999. Effects of free fatty acids on oxidative stability of vegetable oil. J. Am. Oil Chem. Soc. 76 (3), 325-329. https://doi.org/10.1007/s11746-999-0239-4

Jiang S, Xie Y, Li M, Guo Y, Cheng Y, Qian H, Yao W. 2020. Evaluation on the oxidative stability of edible oil by electron spin resonance spectroscopy. Food Chem. 309, 125714. https://doi.org/10.1016/j.foodchem.2019.125714 PMid:31671375

Koprivnjak O, Škevin D, Valić S, Majetić V, Petričević S, Ljubenkov I. 2008. The antioxidant capacity and oxidative stability of virgin olive oil enriched with phospholipids. Food Chem. 111 (1), 121-126. https://doi.org/10.1016/j.foodchem.2008.03.045

Kristensen D, Skibsted LH. 1999. Comparison of three methods based on electron spin resonance spectrometry for evaluation of oxidative stability of processed cheese. J. Agric. Food Chem. 47 (8), 3099-3104. https://doi.org/10.1021/jf981396p PMid:10552615

Lerma-García MJ, Simó-Alfonso EF, Bendini A, Cerretani L. 2011. Rapid evaluation of oxidised fatty acid concentration in virgin olive oil using Fourier-transform infrared spectroscopy and multiple linear regression. Food Chem. 124 (2), 679-684. https://doi.org/10.1016/j.foodchem.2010.06.054

Ottaviani MF, Spallaci M, Cangiotti M, Bacchiocca M, Ninfali P. 2001. Electron paramagnetic resonance investigations of free radicals in extra virgin olive oils. J. Agric. Food Chem. 49 (8), 3691-3696. https://doi.org/10.1021/jf001203+ PMid:11513649

Papadimitriou V, Sotiroudis TG, Xenakis A, Sofikiti N, Stavyiannoudaki V, Chaniotakis NA. 2006. Oxidative stability and radical scavenging activity of extra virgin olive oils: An electron paramagnetic resonance spectroscopy study. Anal. Chim. Acta 573, 453-458. https://doi.org/10.1016/j.aca.2006.02.007 PMid:17723560

Paradiso VM, Pasqualone A, Summo C, Caponio F. (2018). An "omics" approach for lipid oxidation in foods: The case of free fatty acids in bulk purified olive oil. Eur. J. Lipid Sci. Technol. 120 (7), 1800102. https://doi.org/10.1002/ejlt.201800102

Raitio R, Orlien V, Skibsted LH. 2011. Electron spin resonance spectroscopy for evaluation of early oxidative events in semisolid palm oil. Eur. J. Lipid Sci. Technol. 113 (2), 208-213. https://doi.org/10.1002/ejlt.201000087

Ramadan MF, Wahdan KMM. 2012. Blending of corn oil with black cumin (Nigella sativa) and coriander (Coriandrum sativum) seed oils: Impact on functionality, stability and radical scavenging activity. Food Chem. 132 (2), 873-879. https://doi.org/10.1016/j.foodchem.2011.11.054

Raudsepp P, Brüggemann DA, Lenferink A, Otto C, Andersen ML. 2014. Oxidative stabilization of mixed mayonnaises made with linseed oil and saturated medium-chain triglyceride oil. Food Chem. 152, 378-385. https://doi.org/10.1016/j.foodchem.2013.11.141 PMid:24444951

Reboredo-Rodríguez P, Valli E, Bendini A, Di Lecce G, Simal‐Gándara J, Gallina Toschi T. 2016. A widely used spectrophotometric assay to quantify olive oil biophenols according to the health claim (EU Reg. 432/2012). Eur. J. Lipid Sci. Technol. 118 (10), 1593-1599. https://doi.org/10.1002/ejlt.201500313

Ricca M, Foderà V, Vetri V, Buscarino G, Montalbano M, Leone M. 2012. Oxidation processes in Sicilian olive oils investigated by a combination of optical and EPR spectroscopy. J. Food Sci. 77 (10), C1084-C1089. https://doi.org/10.1111/j.1750-3841.2012.02913.x PMid:22957943

Shahidi F, Wanasundara UN. 2002. Methods for measuring oxidative rancidity in fats and oils. In Food lipids: Chemistry, nutrition and biotechnology, 3rd ed.; Akoh, C.C., Min, D.B., Eds; Marcel Dekker Inc., New York, Volume 17, pp. 387-403. https://doi.org/10.1201/9780203908815.ch14

Thomsen MK, Lauridsen L, Skibsted LH, Risbo J. 2005. Two types of radicals in whole milk powder. Effect of lactose crystallization, lipid oxidation, and browning reactions. J. Agric. Food Chem. 53 (5), 1805-1811. https://doi.org/10.1021/jf0485483 PMid:15740077

Tura M, Mandrioli M, Valli E, Rubino RC, Parentela D, Gallina Toschi T. 2022. Changes in the composition of a cold-pressed hemp seed oil during three months of storage. J. Food Compos. Anal. 106, 104270. https://doi.org/10.1016/j.jfca.2021.104270

Velasco J, Andersen ML, Skibsted LH. 2004. Evaluation of oxidative stability of vegetable oils by monitoring the tendency to radical formation. A comparison of electron spin resonance spectroscopy with the Rancimat method and differential scanning calorimetry. Food Chem. 85 (4), 623-632. https://doi.org/10.1016/j.foodchem.2003.07.020

Xie Y, Jiang S, Li M, Guo Y, Cheng Y, Qian H, Yao W. 2019. Evaluation on the formation of lipid free radicals in the oxidation process of peanut oil. LWT 104, 24-29. https://doi.org/10.1016/j.lwt.2019.01.016

Yang J, Qin L, Zhu Y, He C. 2022. The regularity of heat-induced free radicals generation and transition of camellia oil. Food Res. Int. 157, 111295. https://doi.org/10.1016/j.foodres.2022.111295 PMid:35761600

Yi J, Andersen ML, Skibsted LH. 2011. Interactions between tocopherols, tocotrienols and carotenoids during autoxidation of mixed palm olein and fish oil. Food Chem. 127(4), 1792-1797. https://doi.org/10.1016/j.foodchem.2011.02.061

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Published

2025-03-30

How to Cite

1.
Tura M, Mandrioli M, Valli E, Bendini A, Gallina Toschi T. Electron spin resonance (microESR) to determine the peroxide value of virgin olive oil. Grasas aceites [Internet]. 2025Mar.30 [cited 2026Jul.27];76(1):2201. Available from: https://grasasyaceites.revistas.csic.es/index.php/grasasyaceites/article/view/2201

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