Skip to main content
Log in

Determining adulteration of canned products using SNIF-NMR and IRMS: detection of undeclared addition of synthetic acetic acid

  • Original Paper
  • Published:
European Food Research and Technology Aims and scope Submit manuscript

Abstract

Possible adulteration of canned products containing spirit vinegar pickle by adding synthetic acetic acid is a significant problem of the food industry. Isotope analyses, which determine botanical origin of acetic acid and also can detect synthetic acid, were applied to detect undeclared addition of synthetic acetic acid to canned products. The aim of the study was to improve the extraction technique for the SNIF-NMR (2H/1H; site-specific natural isotopic fractionation-nuclear magnetic resonance) and IRMS (13C/12C; isotope ratio mass spectrometry) isotope methods and for an atypical matrix and to determine isotope ratios in canned vegetables pickle to prove their adulteration or authenticity. The following set of canned products was analysed: pickled cucumbers (n = 16) and one vinegar pickle purchased in the Czech market and six model (cucumber) pickles. The determined ratios of 2H/1H and 13C/12C for the pickled cucumbers proved to be authentic ranged from 89.4 to 107.0 ppm and from −28.7 to −15.6 ‰, respectively; for the synthetic acetic acids diluted with water they ranged from 114.2 to 129.0 ppm and from −44.9 to −33.4 ‰, respectively. Isotope analyses were confirmed as a reliable tool for assessing authenticity of canned products. The method enables detection of synthetic acetic acid addition into vinegars and canned vegetables containing vinegar pickle up from 20 % (of total acidity).

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1

Similar content being viewed by others

References

  1. Grégrová A, Čížková H, Mazáč J, Voldřich M (2012) Authenticity assessment of spirit vinegar (part I): production and analysis methods. Kvasný průmysl 58:309–312

    Google Scholar 

  2. European Commission (2012) Commission regulation (EU) No 231/2012 of 9 March 2012 laying down specifications for food additives listed in Annexes II and III to regulation (EC) No 1333/2008 of the European Parliament and of the Council. Off J Eur Union L83:1–295

  3. Ministry of Agriculture of the Czech Republic (1997) Decree No. 335/1997 Coll., implementing Section 18 a), d), h), i), j), and k) of Act No. 110/1997 Coll., on food and tobacco products, and on changes and amendments to certain related acts, for non-alcoholic beverages and concentrates for the preparation of non-alcoholic beverages, fruit wines, other wines and mead, beer, potable alcohol and other alcoholic beverages, vinegar and yeast, as amended. Collection of Laws of the Czech Republic 111/1997:6834–6854

  4. Camin F, Bontempo L, Perini M, Tonon A, Breas O, Guillou C, Moreno-Rojas JM, Gagliano G (2013) Control of wine vinegar authenticity through δ18O analysis. Food Control 29(1):107–111

    Article  CAS  Google Scholar 

  5. Schmid ER, Fogy I, Schwarz P (1978) Beitrag zur Unterscheidung von Gärungsessig und synthetischem Säureessig durch die massenspektrometrische Bestimmung des13C/12-Isotopenverhältnisses. Z. Lebensm. Unters.-Forsch. 166:89–92

    Article  CAS  Google Scholar 

  6. Remaud G, Guillou C, Vallet C, Martin GJ (1992) A coupled NMR and MS isotopic method for the authentication of natural vinegars. Fresenius J Anal Chem 342:457–461

    Article  CAS  Google Scholar 

  7. Hermann A (2001) Determination of D/H isotope ratio in acetic acid from vinegars and pickled products by 2H-NMR-spectroscopy. Eur Food Res Technol 212:683–686

    Article  CAS  Google Scholar 

  8. Caligiani A, Acquotti D, Palla G, Bocchi V (2007) Identification and quantification of the main organic components of vinegars by high resolution 1H NMR spectroscopy. Anal Chim Acta 585:110–119

    Article  CAS  Google Scholar 

  9. Thomas F, Jamin E (2009) 2H NMR and 13C-IRMS analyses of acetic acid from vinegar, 18O-IRMS analysis of water in vinegar: international collaborative study report. Anal Chim Acta 649:98–105

    Article  CAS  Google Scholar 

  10. Meier-Augenstein W (2004) Handbook of stable isotope analytical techniques. Elsevier, Amsterdam

    Google Scholar 

  11. Hattori R, Yamada K, Shibata H, Hirano S, Tajima O, Yoshida N (2010) Measurement of the isotope ratio of acetic acid in vinegar by HS-SPME-GC-TC/C-IRMS. J Agric Food Chem 58(12):7115–7118

    Article  CAS  Google Scholar 

  12. Grégrová A, Čížková H, Mazáč J, Voldřich M (2012) Authenticity and quality of spirit vinegar: methods for detection of synthetic acetic acid addition. J Food Nutr Res 51:123–131

    Google Scholar 

  13. Waterisotopes.org (2003–2013) Gabriel Bowen, University of Utah. http://wateriso.utah.edu/waterisotopes/media/IsoMaps/jpegs/o_Euro/oma_Euro.jpg. Accessed 21 April 2013

  14. ISO 760:1978 Determination of water—Karl Fischer method (general method) (2009). http://www.iso.org/iso/home/store/catalogue_tc/catalogue_detail.htm?csnumber=5037

  15. Kaufmann A (1993) Übersicht und Anwendung der HPLC-Analytik von Säuren und Zucker in Wein. Mitt Gebiete Lebensm Hyg 84:311–333

    CAS  Google Scholar 

  16. European Commission (1990) Commission regulation (EEC) No 2676/90 of 17 September 1990 determining community methods for the analysis of wines. Off J Eur Union L272:1–192

  17. European Commission (2003) Commission regulation (EC) No 440/2003 of 10 March 2003 amending regulation (EEC) No 2676/90 determining community methods for the analysis of wines. Off J Eur Union L66:15–23

  18. European Commission (1997) Commission regulation (EC) No 822/97 of 6 May 1997 amending regulation (EEC) No 2676/90 determining community methods for the analysis of wines. Off J Eur Union L117:10–12

  19. McFeeters RF (1993) Single injection HPLC analysis of acids, sugars, and alcohols in Cucumber fermentations. J Agric Food Chem 41:1439–1443

    Article  CAS  Google Scholar 

  20. Tsuchida H, Kozukue N, Han GP, Choi SH, Levin CE (2010) Low-temperature storage of cucumbers induced changes in the organic acid content and in citrate synthase activity. Postharvest Biol Technol 58:129–134

    Article  CAS  Google Scholar 

  21. Johanningsmeier SD, McFeeters RF (2013) Metabolism of lactic acid in fermented cucumbers by Lactobacillus buchneri and related species, potential spoilage organisms in reduced salt fermentations. Food Microbiol 35:129–135

    Article  CAS  Google Scholar 

  22. Eurodiag 1.1 (2002) An interpretation modul, copyright: Eurofins

Download references

Acknowledgments

Financial support was secured from specific university research (Ministry of Education, Youth and Sports No. 20/2013) and from the Ministry of Agriculture Project No. QI91B283. The authors express thanks to their colleagues from the Customs Technical Laboratory Prague (Petra Majerová and Jitka Velíšková) for their help and cooperation in this project. The authors wish to express their sincere thanks to the late Professor Michal Voldřich for his kind suggestions, encouragement and inspiration not only in this work.

Conflict of interest

None.

Compliance with Ethics Requirements

This article does not contain any studies with human or animal subjects.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Adéla Grégrová.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Grégrová, A., Neradová, E., Kružík, V. et al. Determining adulteration of canned products using SNIF-NMR and IRMS: detection of undeclared addition of synthetic acetic acid. Eur Food Res Technol 239, 169–174 (2014). https://doi.org/10.1007/s00217-014-2209-9

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00217-014-2209-9

Keywords

Navigation