Results of an Interlaboratory Comparison of a Liquid Chromatography-Isotope Ratio Mass Spectrometry Method for the Determination of 13C/12C Ratios of Saccharides in Honey

J AOAC Int. 2021 Dec 11;104(6):1698-1702. doi: 10.1093/jaoacint/qsab091.

Abstract

Background: Stable carbon isotope analysis of sugars in honey by LC-isotope ratio mass spectrometry (IRMS) is a useful tool for detecting adulteration of honey with extraneous sugar. Purity criteria based on 13C/12C ratios of saccharides in honey, determined by LC-IRMS of a large number of authentic honey samples, have been elaborated. However, no interlaboratory comparison (ILC) has yet been performed to estimate the precision of the method under reproducibility conditions.

Objective: To address this knowledge gap an ILC involving 14 laboratories and using six honey samples was conducted.

Methods: The participants were allowed to use their LC-IRMS-based method of choice for sample preparation and compound separation.

Results: The precision figures were estimated according to ISO 5725:1994. The repeatability relative standard deviation (RSDr) for the determination of δ13C values of fructose and glucose varied between 0.3 and 0.5%, with 0.3 and 1.0% for disaccharides, and 0.7 and 2.8% for trisaccharides. The RSDR varied between 0.8 and 1.8% for the monosaccharides, 1.0 and 1.5% for disaccharides, and 1.4 and 2.8% for trisaccharides.

Conclusion: Based on the obtained precision data the LC-IRMS method for the determination of 13C/12C ratios of saccharides in honey was considered fit for the conformity assessment of honey with established purity criteria.

Highlights: Precision estimates for a LC-IRMS method to determine 13C/12C ratios of saccharides in honey were obtained through an ILC. The data created can form the basis for the standardization of the method by interested standards-developing organizations for use in official control.

MeSH terms

  • Carbon Isotopes
  • Chromatography, Liquid
  • Honey* / analysis
  • Humans
  • Mass Spectrometry
  • Reproducibility of Results

Substances

  • Carbon Isotopes
  • Carbon-13