Determination of free fatty acids in edible oils by <sup>1</sup>H NMR spectroscopy

Skiera, Christina; Steliopoulos, Panagiotis; Kuballa, Thomas; Holzgrabe, Ulrike; Diehl, Bernd

doi:10.1002/lite.201200241

Cited by 43 publications

(30 citation statements)

References 6 publications

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“…1 H NMR spectroscopy was also applied to determine the AV of vegetable oils such as olive and sunflower oil as well as cod liver oil by Skiera et al . These researchers used the signal area of the C 2 methylene group between 2.2 and 2.4 ppm and the integrated singlet of the free carboxyl group between 11 and 12 ppm in order to quantify free fatty acids in mmol/mol triglycerides.…”

Section: Discussionmentioning

confidence: 99%

Toward determining fat quality parameters of fish oil by means of ¹H NMR spectroscopy

Giese¹,

Winkelmann

Rohn³

et al. 2016

Euro J Lipid Sci & Tech

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The consumption of fish oil-based dietary supplements has increased dramatically in recent years, which is mainly due to their high content of health promoting omega-3 fatty acids. However, these polyunsaturated fatty acids are extremely prone to oxidation. This study investigated the potential of 1 H NMR spectroscopy for the assessment of the oxidative deterioration of fish oils. Nine raw fish oils of different fish species were stored for 3 months at room temperature at different degrees of sunlight exposure as well as under standardized accelerated storage conditions for 6 days (at 40°C and under constant light exposure). Fish oil samples were analyzed by 1 H NMR spectroscopy as well as by traditional methods to determine the fat quality parameters peroxide value (PV), anisidine value (AnV), TOTOX value, and acid value (AV). PLS (partial least squares) regression models were used to predict these fat quality parameters based on the 1 H NMR spectra. The best regression models reached an R 2 of 0.949, 0.962, 0.991, and 0.977 for PV, AnV, TOTOX value, and AV, respectively. In conclusion, 1 H NMR spectroscopy is a promising approach for a fast, reliable, and sustainable assessment of fish oil quality with regard to lipid oxidation. Practical applications:The results indicate a great potential of 1 H NMR spectroscopy in the quality assessment of fish oils. This technology requires little time, work, amount of sample, and solvent and provides extensive information that can be obtained from a single spectrum. Such an approach is significantly more specific and detailed than traditional lipid oxidation parameters.

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Section: Discussionmentioning

confidence: 99%

Toward determining fat quality parameters of fish oil by means of ¹H NMR spectroscopy

Giese¹,

Winkelmann

Rohn³

et al. 2016

Euro J Lipid Sci & Tech

View full text Add to dashboard Cite

show abstract

“…Unlike other techniques, such as GC or HPLC, derivatization and pretreatment of a lipid sample is not necessary for NMR analysis, and it has been proven to be a reliable quantitative method. NMR has also been compared to several standard methods typically used to study oxidative degradation of oil and lipid samples, including PV, conjugated diene and triene contents, PAV, TBARS, and acid value (Shahidi and others ; Wanasundara and others ; Skiera and others , b). Good correlation was reported between NMR and the standard methods, suggesting that NMR was an effective way to determine both primary and secondary oxidation products.…”

Section: Nmr Spectroscopymentioning

confidence: 99%

Techniques for the Analysis of Minor Lipid Oxidation Products Derived from Triacylglycerols: Epoxides, Alcohols, and Ketones

Xia

Budge

2017

Comp Rev Food Sci Food Safe

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Lipid oxidation can lead to flavor and safety issues in fat-containing foods. In order to measure the extent of lipid oxidation, hydroperoxides and their scission products are normally targeted for analytical purposes. In recent years, the formation of rarely monitored oxygenated products, including epoxides, alcohols, and ketones, has also raised concerns. These products are thought to form from alternative pathways that compete with chain scissions, and should not be neglected. In this review, a number of instrumental techniques and approaches to determine epoxides, alcohols, and ketones are discussed, with a focus on their selectivity and sensitivity in applications to food lipids and oils. Special attention is given to methods employing gas chromatography (GC), high-performance liquid chromatography (HPLC), and nuclear magnetic resonance (NMR). For characterization purposes, GC-mass spectrometry (GC-MS) provides valuable information regarding the structures of individual oxygenated fatty acids, typically as methyl esters, isolated from oxygenated triacylglycerols (TAGs), while the use of liquid chromatography-MS (LC-MS) techniques allows analysis of intact oxygenated TAGs and offers information about the position of the oxygenated acyl chain on the glycerol backbone. For quantitative purposes, traditional chromatography methods have exhibited excellent sensitivity, while spectroscopic methods, including NMR, are superior to chromatography for their rapid analytical cycles. Future studies should focus on the development of a routine quantitative method that is both selective and sensitive.

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“…For instance, short-chain FFA can arise from the secondary oxidation of unsaturated aldehydes as well as from the cleavage of lipid hydroperoxides [1,2]. The FFA concentration in vegetable oils depends on multiple factors, namely the quality and variety of raw material, collecting conditions, processing, storage, the age of the oil and deterioration status [3,4]. The amount of FFA is even higher in waste cooking oils (WCO), since high temperature and exposure to air occurring during frying promote the hydrolysis and oxidation of triglycerides and increase the content of FFA in the oil [5][6][7][8].…”

Section: Introductionmentioning

confidence: 99%

NMR Determination of Free Fatty Acids in Vegetable Oils

2020

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The identification and quantification of free fatty acids (FFA) in edible and non-edible vegetable oils, including waste cooking oils, is a crucial index to assess their quality and drives their use in different application fields. NMR spectroscopy represents an alternative tool to conventional methods for the determination of FFA content, providing us with interesting advantages. Here the approaches reported in the literature based on 1H, 13C and 31P NMR are illustrated and compared, highlighting the pros and cons of the suggested strategies.

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Determination of free fatty acids in edible oils by ¹H NMR spectroscopy

Cited by 43 publications

References 6 publications

Toward determining fat quality parameters of fish oil by means of ¹H NMR spectroscopy

Toward determining fat quality parameters of fish oil by means of ¹H NMR spectroscopy

Techniques for the Analysis of Minor Lipid Oxidation Products Derived from Triacylglycerols: Epoxides, Alcohols, and Ketones

NMR Determination of Free Fatty Acids in Vegetable Oils

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Determination of free fatty acids in edible oils by 1H NMR spectroscopy

Cited by 43 publications

References 6 publications

Toward determining fat quality parameters of fish oil by means of 1H NMR spectroscopy

Toward determining fat quality parameters of fish oil by means of 1H NMR spectroscopy

Techniques for the Analysis of Minor Lipid Oxidation Products Derived from Triacylglycerols: Epoxides, Alcohols, and Ketones

NMR Determination of Free Fatty Acids in Vegetable Oils

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Determination of free fatty acids in edible oils by ¹H NMR spectroscopy

Toward determining fat quality parameters of fish oil by means of ¹H NMR spectroscopy

Toward determining fat quality parameters of fish oil by means of ¹H NMR spectroscopy