Stable Isotope Ratio Determination of the Origin of Vanillin in Vanilla Extracts and Its Relationship to Vanillin/Potassium Ratios

Martin, Glenn E; Alfonso, Felipe C; Figert, Donald M; Burggraff, James M

doi:10.1093/jaoac/64.5.1149

Cited by 4 publications

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“…Although the intramolecular variability seems to be exaggerated by systematic biases, the NMR method is able to characterize the three kinds of samples on a relative basis. The observed behaviors are in reasonable agreement with some partial determinations performed by mass spectrometry on degradation products of vanillin (34)(35)(36).…”

Section: Definitions and Symbolssupporting

confidence: 88%

Determination of site-specific carbon isotope ratios at natural abundance by carbon-13 nuclear magnetic resonance spectroscopy

Caer

Trierweiler²,

Martin³

et al. 1991

Anal. Chem.

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Site-specific natural isotope fractionation of hydrogen studied by deuterium NMR (SNIF-NMR) spectroscopy is a powerful source of information on hydrogen pathways occurring in biosyntheses in natural conditions. The potential of the carbon counterpart of this method has been investigated and compared. Three typical molecular species, ethanol, acetic acid, and vanillin, have been considered. Taking into account the requirements of quantitative 13C NMR, appropriate experimental procedures have been defined and the repeatability and reproducibility of the isotope ratio determinations have been checked in different conditions. It is shown that the carbon version of the SNIF-NMR method is capable of detecting small differences in the carbon-13 content of the ethyl fragment of ethanols from different botanical or synthetic origins. These results are in agreement with mass spectrometry determinations of the overall carbon isotope ratios. Deviations with respect to a statistical distribution of 13C have been detected in the case of acetic acid and vanillin. However, since the method is very sensitive to several kinds of systematic error, only a relative significance can be attached at present to the internal parameters directly accessible. Isotope dilution experiments have also been carried out in order to check the consistency of the results. In the present state of experimental accuracy, the 13C NMR method is of more limited potential than 2H SNIF-NMR spectroscopy. However it may provide complementary information. Moreover it is particularly efficient for detecting and quantifying adulterations that aim to mimic the overall carbon-13 content of a natural compound by adding a selectivity enriched species to a less expensive substrate from a different origin.

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Section: Definitions and Symbolssupporting

confidence: 88%

Determination of site-specific carbon isotope ratios at natural abundance by carbon-13 nuclear magnetic resonance spectroscopy

Caer

Trierweiler²,

Martin³

et al. 1991

Anal. Chem.

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“…One of the oldest methods (1981) used for isotope‐ratio mass spectrometry (IRMS) is thin‐layer chromatography (TLC). [4] Because the vanillin band is scraped off the TLC plate, this does not offer real control of the quantitative analyte recovery and does not allow automation.…”

Section: Introductionmentioning

confidence: 99%

“…However, the recoveries were limited to less than 5 mg per injection,[10,11] which is enough for IRMS analysis, but insufficient for quantitative NMR. An interlaboratory test was made in 1982[12] to validate the sample preparation step prior to IRMS, using preparative GC[10] and TLC;[4] both gave satisfactory results.…”

Section: Introductionmentioning

confidence: 99%

Procedure for the isolation of vanillin from vanilla extracts prior to isotopic authentication by quantitative ¹³C‐NMR

Cicchetti¹,

Silvestre²,

Fieber³

et al. 2010

Flavour & Fragrance J

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Quantitative isotopic 13 C-NMR at natural abundance recently became a new tool for the authentication of natural flavours. In contrast to isotopic-ratio mass spectrometry, which yields the global 13 C/ 12 C ratio of a molecule, isotopic 13 C-NMR allows the determination of isotopic ratios of each spectroscopically differentiable carbon site. Since it requires a significant amount of the purified analyte, an optimized vanillin isolation procedure is presented here. It involves an accelerated solvent extraction of beans, a fat removal step and a subsequent medium-pressure isolation of the vanillin peak on a reusable reverse-phase column, using mostly water as a mobile phase (97%). The overall recovery from the bean extract is 90%. The procedure was automated as much as possible and checked against the risk of isotopic fractionation. The overall protocol was demonstrated to be suitable for isotopic measurements.

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“…The problem is compounded by the additional need to distinguish "nature-identical" from synthetic sources (3). Three basic approaches to resolving this problem have been taken: ash analysis (4), compositional profiling (5,6), and isotopic profiling (4,(6)(7)(8)(9)(10)(11)(12). Of these, the use of isotopic analysis has proved to be the most effective.…”

Section: Introductionmentioning

confidence: 99%

Authentication of the Origin of Vanillin Using Quantitative Natural Abundance ¹³C NMR

Tenailleau

Lancelin

Robins

et al. 2004

J. Agric. Food Chem.

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The use of 13C isotopic distribution as an efficient means to determine the origin of vanillin has been substantiated. Using quantitative 13C NMR, the 13C/12C ratios at all eight carbon positions can be exploited. On a set of 21 samples of vanillin from five different origins, complete discrimination can be achieved. It is shown that, for many purposes, a rapid analysis in which only five sites are used is sufficient. However, improved discrimination using all eight sites is preferable to differentiate between different methods of production from natural ferulic acid or between natural and lignin-derived vanillin on the basis of the 13C/12C ratios characteristic of different origins. The C1 and C8 positions are demonstrated to be the most significant sites for discrimination using principle component analysis. However, aromatic carbon positions make an essential contribution, notably in differentiating between natural and lignin-derived vanillin.

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Stable Isotope Ratio Determination of the Origin of Vanillin in Vanilla Extracts and Its Relationship to Vanillin/Potassium Ratios

Cited by 4 publications

References 0 publications

Determination of site-specific carbon isotope ratios at natural abundance by carbon-13 nuclear magnetic resonance spectroscopy

Determination of site-specific carbon isotope ratios at natural abundance by carbon-13 nuclear magnetic resonance spectroscopy

Procedure for the isolation of vanillin from vanilla extracts prior to isotopic authentication by quantitative ¹³C‐NMR

Authentication of the Origin of Vanillin Using Quantitative Natural Abundance ¹³C NMR

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Stable Isotope Ratio Determination of the Origin of Vanillin in Vanilla Extracts and Its Relationship to Vanillin/Potassium Ratios

Cited by 4 publications

References 0 publications

Determination of site-specific carbon isotope ratios at natural abundance by carbon-13 nuclear magnetic resonance spectroscopy

Determination of site-specific carbon isotope ratios at natural abundance by carbon-13 nuclear magnetic resonance spectroscopy

Procedure for the isolation of vanillin from vanilla extracts prior to isotopic authentication by quantitative 13C‐NMR

Authentication of the Origin of Vanillin Using Quantitative Natural Abundance 13C NMR

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Product

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Procedure for the isolation of vanillin from vanilla extracts prior to isotopic authentication by quantitative ¹³C‐NMR

Authentication of the Origin of Vanillin Using Quantitative Natural Abundance ¹³C NMR