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. 2022 Aug 19;2(8):1237-1242.
doi: 10.1021/acsfoodscitech.2c00057. Epub 2022 Jul 11.

Improved Quantification by Nuclear Magnetic Resonance Spectroscopy of the Fatty Acid Ester Composition of Extra Virgin Olive Oils

Affiliations

Improved Quantification by Nuclear Magnetic Resonance Spectroscopy of the Fatty Acid Ester Composition of Extra Virgin Olive Oils

Gabriel Rossetto et al. ACS Food Sci Technol. .

Abstract

Analysis of foods, which are typically highly complex mixtures, by 1H NMR can be difficult because the prevalence of signal overlap complicates characterization and quantification. The various components of a food sample may have a wide range of concentrations, leading to a high dynamic range NMR spectrum and complicating the analysis of less concentrated species. One source of this complication is the presence of 13C satellites, peaks that appear either side of a parent peak with ∼0.56% of its intensity. Satellites of concentrated species can easily be comparable in intensity to the signals of minor components, and can partly or wholly obscure them. This is commonly seen in olive oil samples, leading to inaccurate calculation of the fatty acid ester composition of the oil, used for determining the quality of edible oils and for detecting adulteration. Here, we show that the recently introduced Destruction of Interfering Satellites by Perfect Echo Low-pass filtration (DISPEL) experiment is able to suppress 13C satellites and can substantially improve the accuracy of integration of minor signals. The DISPEL experiment does not require any complicated optimization, working "out of the box" with standard parameters, and incurs no significant loss of sensitivity. It has the potential to become the default experiment, replacing conventional 1D 1H NMR, for quantitative analysis of olive oil.

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Conflict of interest statement

The authors declare no competing financial interest.

Figures

Figure 1
Figure 1
500 MHz (a) conventional 1H NMR and (b) DISPEL spectra for sample EVOO1 with signals assigned to a glycerol unit and the fatty acid chains of palmitic, oleic, and linolenic acids. Panels (c) and (d) are vertical expansions of panels (a) and (b), respectively, showing the spectral region around A and B. The overlap of the 13C satellite of A with B is seen in panel (c), with the removal of the 13C satellites by DISPEL in panel (d), which allows for signal B to be more accurately integrated.

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