Abstract1H NMR spectra of 66 samples of edible oils from 14 different botanical origins were acquired. Assignment of signal spectra to the different types of hydrogen atoms was made and the areas of the signals determined. Considering that the area of the signals of the spectra is proportional to the number of hydrogen atoms of each type in the sample, it is possible to calculate not only the iodine value, but also the proportion of different acyl groups from the data. Determination of both parameters requires only a few minutes and one spectroscopic run. Classical methodology however, requires two separate wet methods for determining the unsaturation degree (iodine value) and the proportions of different acyl groups; both of them involve chemical transformations of the sample and considerable time and cost. Determination of acyl group proportions in samples by 1H NMR, which was validated with mixtures of standard triglycerides, provides accurate results and is able to detect small differences between samples of very similar composition.
The static headspace composition of sunflower oil throughout the oxidation process at 70 degrees C with circulating air is studied by means of solid-phase microextraction followed by gas chromatography-mass spectrometry (SPME-GC-MS); at the same time the liquid phase of the same oil is studied by means of Fourier transform infrared (FTIR) spectroscopy. Each technique provides complementary information about the process; FITR spectroscopy detects changes in the functional groups of the liquid matrix in a global way and SPME/GC-MS provides information about the different components present in the volatile phase during the oxidation process. Concordance between the timing of the changes produced in both liquid and gaseous phases is observed, as well as agreement and complementarity in the results obtained from both phases. The formation of some well-known genotoxic and cytotoxic oxygenated aldehydes in this process and their presence in the oil headspace are proved.
Several samples containing different proportions of standard compounds such as tristearin, triolein, trilinolein, and trilinolenin, covering a broad range of compositions, some similar to those of edible oils, were prepared by weight. The 1H nuclear magnetic resonance (NMR) spectra of these samples were recorded and their signals were assigned. It was shown that concentrations of linolenic acyl groups close to 0.4% or higher can be detected by this technique. The area of 5 discrete proton signals of the spectrum was determined. Considering the ratio between this area and the concentration of the corresponding types of hydrogen atoms in the sample, equations calculating the proportions of the acyl groups were deduced. The high level of agreement between data coming from 1H NMR spectra and data obtained by weight shows the usefulness of this methodology. In addition, it has the advantage that it is very fast and simple in comparison with the classical methods, and does not require a chemical modification of the sample. For this reason, the described method constitutes a valuable alternative for the determination of the proportions of different acyl groups in acylglycerol mixtures, such as, for example, oils and fats.
Three oil samples obtained from sacha inchi (Plukenetia volubilis L.) seeds were studied by means of FTIR and 1 H NMR. Frequency data of the most significant bands of the IR spectrum of this oil are given. These data show that sacha inchi oil has a high degree of unsaturation. The same fact is deduced from the ratio between the absorbance of the bands due to the stretching vibrations of the cis olefinic CH double bonds at 3010.5 cm −1 and to the methylene symmetrical stretching vibrations at 2855.1 cm −1 . The proportions of monounsaturated, polyunsaturated, and saturated acyl groups were predicted from the frequency of some IR bands, and these were in satisfactory agreement with the values obtained through FAME generation and their quantification by GC. Likewise, simple observation of the 1 H NMR spectra provided a great deal of information about sacha inchi oil, with regard not only to the relative proportions of the different acyl groups but also to their nature. Thus, the presence of γ-linolenic acyl groups was discounted. Furthermore, the area of some 1 H NMR signals was used to determine the proportion of saturated and mono-, di-, and triunsaturated acyl groups, which also were in satisfactory agreement with the values obtained by classical methods. IR and 1 H NMR determinations take very little time in comparison with classical methods and do not require chemical manipulation or transformation of the sample. A comparison was also made between the compositions of sacha inchi and linseed oil. Both oils are important sources of the healthful n-3 linolenic acyl groups, and sacha inchi also contains high proportions of the n-6 linoleic acyl groups.Paper no. J10400 in JAOCS 80, 755-762 (August 2003).
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