Rapid and Direct Low Micromolar NMR Method for the Simultaneous Detection of Hydrogen Peroxide and Phenolics in Plant Extracts

A rapid and direct low micromolar 1H NMR method for the simultaneous identification and quantification of hydrogen peroxide and phenolic compounds in plant extracts was developed. The method is based on the highly deshielded 1H NMR signal of H2O2 at ∼10.30 ppm in DMSO-d 6 and the combined use of pic...

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Bibliographic Details
Published in:Journal of agricultural and food chemistry 2012-05, Vol.60 (18), p.4508-4513
Main Authors: Charisiadis, Pantelis, Tsiafoulis, Constantinos G, Exarchou, Vassiliki, Tzakos, Andreas G, Gerothanassis, Ioannis P
Format: Article
Language:English
Subjects:
Biological and medical sciences
Cinnamates - analysis
detection limit
Flavonoids - analysis
Food industries
freezing point
Fundamental and applied biological sciences. Psychology
General aspects
hydrogen peroxide
Hydrogen Peroxide - analysis
Magnetic Resonance Spectroscopy - methods
Methods of analysis, processing and quality control, regulation, standards
Microchemistry - methods
Monoterpenes - analysis
nuclear magnetic resonance spectroscopy
oregano
Origanum - chemistry
phenolic compounds
Phenols - analysis
Plant Components, Aerial - chemistry
plant extracts
Plant Extracts - chemistry
temperature
Time Factors
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Summary:A rapid and direct low micromolar 1H NMR method for the simultaneous identification and quantification of hydrogen peroxide and phenolic compounds in plant extracts was developed. The method is based on the highly deshielded 1H NMR signal of H2O2 at ∼10.30 ppm in DMSO-d 6 and the combined use of picric acid and low temperature, near the freezing point of the solution, in order to achieve the minimum proton exchange rate. Line widths of H2O2 below 3.8 Hz were obtained for several Greek oregano extracts which resulted in a detection limit of 0.7 μmol L–1. Application of an array of NMR experiments, including 2D 1H–13C HMBC, spiking of the samples with H2O2, and variable temperature experiments, resulted in the unequivocal assignment of H2O2 precluding any confusion with interferences from intrinsic phenolics in the extract.
ISSN:0021-8561
1520-5118
DOI:10.1021/jf205003e