Study and validity of 13C stable carbon isotopic ratio analysis by mass spectrometry and 2H site-specific natural isotopic fractionation by nuclear magnetic resonance isotopic measurements to characterize and control the authenticity of honey.

Honey samples were analyzed by stable carbon isotopic ratio analysis by mass spectrometry (SCIRA-MS) and site-specific natural isotopic fractionation measured by nuclear magnetic resonance (SNIF-NMR) to first determine their potentials for characterizing the substance and then to combat adulteration. Honey samples from several geographic and botanical origins were analyzed. The delta(13)C parameter was not significant for characterizing an origin, while the (D/H)(I) ratio could be used to differentiate certain single-flower varieties. Application of the official control method of adding a C(4) syrup (AOAC official method 998.12) to our authentic samples revealed anomalies resulting from SCIRA indices that were more negative than -1 per thousand (permil). A filtration step was added to the experimental procedure and provided results that were compliant with the natural origin of our honey samples. In addition, spiking with a C(4) syrup could be detected starting at 9-10%. The use of SNIF-NMR is limited by the detection of a syrup spike starting only at 20%, which is far from satisfying.

[1]  M. Grenier-loustalot,et al.  Application of carbohydrate analysis to verify honey authenticity. , 2003, Journal of chromatography. A.

[2]  J. White,et al.  Stable carbon isotope ratio analysis of honey: validation of internal standard procedure for worldwide application , 1998 .

[3]  Andreas Rossmann,et al.  Improved detection of sugar addition to apple juices and concentrates using internal standard 13C IRMS , 1997 .

[4]  G. Martin,et al.  Detection of Sophisticated Adulterations of Natural Vanilla Flavors and Extracts: Application of the SNIF-NMR Method to Vanillin and p-Hydroxybenzaldehyde , 1997 .

[5]  J. S. Bonvehí,et al.  Determination of stable carbon isotope ratio δ13 C by mass spectrometry in Spanish honeys/Análisis del índice isotópico estable δ13C en mieles españolas mediante resonancia magnética nuclear , 1995 .

[6]  M. Grenier-loustalot,et al.  Chromatographic analysis of sugars applied to the characterisation of monofloral honey , 2004, Analytical and bioanalytical chemistry.

[7]  M. Danzart,et al.  Deuterium nuclear magnetic resonance spectroscopy and stable carbon isotope ratio analysis/mass spectrometry of certain monofloral honeys. , 2000, Journal of AOAC International.

[8]  Harro A. J. Meijer,et al.  Adulteration of honey: relation between microscopic analysis and $\delta^{13}$C measurements , 2000 .

[9]  J. Koziet,et al.  Determination of the oxygen-18 and deuterium content of fruit and vegetable juice water. An European inter-laboratory comparison study , 1995 .

[10]  G. Martin,et al.  Deuterium transfer in the bioconversion of glucose to ethanol studied by specific isotope labeling at the natural abundance level , 1986 .

[11]  L. Doner,et al.  Carbon-13/Carbon-12 Ratio Is Relatively Uniform Among Honeys , 1977, Science.

[12]  N. Naulet,et al.  Application of 2H SNIF-NMR and 13C SIRA-MS analyses to maple syrup: detection of added sugars , 1996 .

[13]  I. Martı́n,et al.  Detection of honey adulteration with beet sugar using stable isotope methodology , 1998 .

[14]  J. Koziet,et al.  Site-specific natural isotópe fractionation in fruit juices determined by deuterium NMR an European inter-laboratory comparison study , 1996 .

[15]  Claude Guillou,et al.  Natural factors of isotope fractionation and the characterization of wines , 1988 .

[16]  P. Morales,et al.  Carbon isotopic composition of Mexican honey , 1997 .

[17]  P. Lindner,et al.  Characterization of Citrus Honey by Deuterium NMR , 1996 .

[18]  Jonathan W. White Internal Standard Stable Carbon Isotope Ratio Method for Determination of C-4 Plant Sugars in Honey: Collaborative Study, and Evaluation of Improved Protein Preparation Procedure , 1992 .

[19]  J. Koziet,et al.  Control of the authenticity of orange juice by isotopic analysis , 1987 .