Skip to main content
Log in

Preliminary LC-IRMS Characterization of Italian Pure Lemon Juices and Evaluation of Commercial Juices Distributed in the Italian Market

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

LC-IRMS determinations of the δ13C values for organic acids and sugars in 20 genuine lemon juices squeezed in the laboratory were obtained from fruits derived from two producer regions of Italy (Campania and Sicily). These samples were used to deduce four ratios to use as indices of the natural variation of these compounds in Italian lemon juice. The corresponding confidence limits were also determined. According to EU laws, addition of acidifying agents to lemon juice is allowed and must be declared on the label, while addition of exogenous sugars is not permitted. We have used the four indices to identify the exogenous addition of these organic compounds to 42 samples of commercial juice lemon distributed on the market. Due to more positive values of δ13C produced by addition of citric acid and sugar from sources with C4-type metabolism, the four judgment ratios permitted us to identify the addition of citric acid and sugars. A nonquantitative method for determination of added compounds is needed, and these LC-IRMS measurements permitted us to obtain the status of the most common additions made to lemon juices in the Italian market.

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.

Fig. 1
Fig. 2

Similar content being viewed by others

References

  • Antolovich M, Li X, Robards K (2001) Detection of adulteration in Australian orange juices by stable carbon isotope ratio analysis (SCIRA). J Agric Food Chem 49:2623–2626

    Article  CAS  Google Scholar 

  • Bahar B, Schmidt O, Moloney AP, Scrimgeour CM, Begley IS, Monahan FJ (2008) Seasonal variation in the C, N and S stable isotope composition of retail organic and conventional Irish beef. Food Chem 106:1299–1305

    Article  CAS  Google Scholar 

  • Boner M, Forstel H (2004) Stable isotope variation as a tool to trace the authenticity of beef. Anal Bioanal Chem 378:301–310

    Article  CAS  Google Scholar 

  • Bononi M, Quaglia G, Tateo F (2015) Easy extraction method to evaluate δ13C vanillin by liquid chromatography-isotopic ratio mass spectrometry in chocolate bars and chocolate snack foods. J Agric Food Chem 63:4777–4781

    Article  CAS  Google Scholar 

  • Brescia MA, Martino GD, Guillou C, Reniero F, Sacco A, Serra F (2002) Differentiation of the geographical origin of durum wheat semolina samples on the basis of isotopic composition. Rapid Commun Mass Spectrom 16:2286–2290

    Article  CAS  Google Scholar 

  • Cabañero AI, Recio JL, Rupérez M (2006) Liquid chromatography coupled to isotope ratio mass spectrometry: a new perspective on honey adulteration detection. J Agric Food Chem 54:9719–9727

    Article  Google Scholar 

  • Cabañero AI, Recio JL, Rupérez M (2008) Isotope ratio mass spectrometry coupled to liquid and gas chromatography for wine ethanol characterization. Rapid Commun Mass Spectrom 22:3111–3118

    Article  Google Scholar 

  • Cabañero AI, Recio JL, Rupérez M (2010) Simultaneous stable carbon isotopic analysis of wine glycerol and ethanol by liquid chromatography coupled to isotope ratio mass spectrometry. J Agric Food Chem 58:722–728

    Article  Google Scholar 

  • Camin F, Bontempo L, Ziller L, Piangiolino C, Morchio G (2010a) Stable isotope ratios of carbon and hydrogen to distinguish olive oil from shark squalene–squalane. Rapid Commun Mass Spectrom 24:1810–1816

    Article  CAS  Google Scholar 

  • Camin F, Larcher R, Nicolini G, Bontempo L, Bertoldi D, Perini M, Schlicht C, Schellenberg A, Thoma F, Heinrich K, Voerkelius S, Horacek M, Ueckermann H, Froeschl H, Wimmer B, Heiss G, Baxter M, Rossmann A, Hoogerwerff J (2010b) Isotopic and elemental data for tracing the origin of European olive oils. J Agric Food Chem 58:570–577

    Article  CAS  Google Scholar 

  • Chabreyrie D, Chauvet S, Guyon F, Salagoïty MH, Antinelli JF, Medina B (2008) Characterization and quantification of grape variety by means of shikimic acid concentration and protein in still white wines. J Agric Food Chem 56:6785–6790

    Article  CAS  Google Scholar 

  • Crittenden RG, Andrew AS, Lefournour M, Young MD, Middleton H, Stockmann R (2007) Determining the geographic origin of milk in Australasia using multi-element stable isotope ratio analysis. Int Dairy J 17:421–428

    Article  CAS  Google Scholar 

  • Di Paola-Naranjo RD, Baroni MV, Podio NS, Rubinstein HR, Fabani MP, Badini RG, Inga M, Ostera HA, Cagnoni M, Gallegos E, Gautier E, Peral-Garcia P, Hoogewerff J, Wunderlin DA (2011) Fingerprints for main varieties of Argentinean wines: terroir differentiation by inorganic, organic, and stable isotopic analyses coupled to chemometrics. J Agric Food Chem 59:7854–7865

    Article  Google Scholar 

  • Directive (EU) 2012 (http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2012:115:0001:0011:EN:PDF)

  • Doner LW (1985) Carbon isotope ratios in natural and synthetic citric acid as indicators of lemon juice adulteration. J Agric Food Chem 33:770–772

    Article  CAS  Google Scholar 

  • Elflein L, Raezke KP (2008) Improved detection of honey adulteration by measuring differences between 13C/12C stable carbon isotope ratios of protein and sugar compounds with a combination of elemental analyzer-isotope ratio mass spectrometry (δ13C-EA/LC-IRMS). Apidologie 39:574–587

    Article  CAS  Google Scholar 

  • Figueira R, Nogueira AM, Ducatt C, Venturini Filho WG, Mischan MM, Da Silva ET (2011) Isotopic analysis (δ13C) method and legal limit in orange nectar. Braz J Food Technol Campinas 14:211–219

    Article  CAS  Google Scholar 

  • Figueira R, Venturini Filho WG, Ducatt C (2013) Carbon isotope analysis in apple nectar beverages. Food Sci Technol Campinas 33:32–37

    Article  Google Scholar 

  • Godin JP, MCCullagh JSO (2011) Review: Current applications and challenges for liquid chromatography coupled to isotope ratio mass spectrometry (LC/IRMS). Rapid Commun Mass Spectrom 25:3019–3028

    Article  CAS  Google Scholar 

  • Gonzalez J, Jamin E, Remaud G, Martin YL, Martin GG, Martin ML (1998) Authentication of lemon juices and concentrates by a combined multi-isotope approach using SNIF-NMR and IRMS. J Agric Food Chem 46:2200–2205

    Article  CAS  Google Scholar 

  • Guyon F, Gaillard L, Salagoïty MH, Medina B (2011) Intrinsic ratios of glucose, fructose, glycerol, and ethanol 13C/12C isotopic ration determined by HPLC-co-IRMS: toward determining constants for wine authentication. Anal Bioanal Chem 401:1551–1558

    Article  Google Scholar 

  • Guyon F, Gaillard L, Brault A, Gaultier N, Salagoïty MH, Medina B (2013) Potential of ion chromatography coupled to isotope ratio mass spectrometry via a liquid interface for beverages authentication. J Chromatogr A 1332:62–68

    Article  Google Scholar 

  • Guyon F, Auberger P, Gaillard L, Loublanches C, Viateau M, Sabathié N, Salagoïty MH, Medina B (2014) 13C/12C isotope ratios of organic acids, glucose and fructose determined by HPLC-co-IRMS for lemon juices authenticity. Food Chem 146:36–40

    Article  CAS  Google Scholar 

  • Jamin E, Gonzales J, Remaud G, Naulet N, Martin GG, Weber D, Rossmann A, Schmidt HL (1997) Improved detection of sugar addition to apple juices and concentrates using internal standard 13C IRMS. Anal Chim Acta 347:359–368

    Article  CAS  Google Scholar 

  • Jamin E, Gonzalez J, Bengoechea I, Kerneur G, Remaud G (1998) Measurement of 13C/12C ratios of sugars, malic acid, and citric acid as authenticity probes of citrus juices and concentrates. J AOAC Int 81:604–609

    CAS  Google Scholar 

  • Jamin E, Guérin R, Retif M, Lees M, Martin GJ (2003) Improved detection of added water in orange juice by simultaneous determination of the oxygen-18/oxygen-16 isotope ratios of water and ethanol derived from sugars. J Agric Food Chem 51:5202–5206

    Article  CAS  Google Scholar 

  • Jamin E, Martin F, Santamaria-Fernandez R, Lees M (2005) Detection of exogenous citric acid in fruit juice by stable isotope ratio analysis. J Agric Food Chem 53:5130–5133

    Article  CAS  Google Scholar 

  • Kelly S, Heaton K, Hoogerwerff J (2005) Tracing the geographical origin of food: the application of multi-element and multi-isotope analysis. Trends Food Sci Technol 16:555–567

    Article  CAS  Google Scholar 

  • Krummen M, Hilkert AW, Juchelka D, Duhr A, Schulter HJ, Pesch R (2004) A new concept for isotope ratio monitoring liquid chromatography/mass spectrometry. Rapid Commun Mass Spectrom 18:2260–2266

    Article  CAS  Google Scholar 

  • Magdas DA, Vedeanu NS, Bolojan L, Puscas R, Damian G (2011) Comparative study between single strength juices and commercial natural juices by IRMS and EPR. Studia UBB Chemia 56:19–27

    CAS  Google Scholar 

  • Molkentin J, Giesemann A (2007) Differentiation of organically and conventionally produced milk by stable isotope and fatty acid analysis. Anal Bioanal Chem 388:297–305

    Article  CAS  Google Scholar 

  • Nakashita R, Suzuki Y, Akamatsu F, Iizumi Y, Korenaga T, Chikaraishi Y (2008) Stable carbon, nitrogen, and oxygen isotope analysis as a potential tool for verifying geographical origin of beef. Anal Chim Acta 617:148–152

    Article  CAS  Google Scholar 

  • Nordic Committee on Food Analysis (NMKL) (1997) Estimation and expression of measurement uncertainty in chemical analysis. NMKL, Oslo, NMKL Procedure 5

    Google Scholar 

  • Ogrinc N, Kosir IJ, Kocjancic M, Kidric J (2001) Determination of authenticity, regional origin, and vintage of Slovenian wines using a combination of IRMS and SNIF-NMR analyses. J Agric Food Chem 49:1432–1440

    Article  CAS  Google Scholar 

  • Ogrinc N, Bat K, Kośir IJ, Golob T, Kokkinofta R (2009) Characterization of commercial Slovenian and Cypriot fruit juices using stable isotopes. J Agric Food Chem 57:6764–6769

    Article  CAS  Google Scholar 

  • Regulation (EC) 2008 (http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32008R1333&from=EN)

  • Regulation (EC) 2011 (https://www.fsai.ie/uploadedFiles/Reg1169_2011.pdf)

  • Suzuky Y, Chikaraishi Y, Ogawa NO, Ohkouchi N, Korenaga T (2008) Geographical origin of polished rice based on multiple element and stable isotope analyses. Food Chem 109:470–475

    Article  Google Scholar 

  • Thomas F, Jamin E, Hammond D (2013) 18O internal referencing method to detect water addition in wines and fruit juices: interlaboratory study. J AOAC Int 96:615–624

    Article  CAS  Google Scholar 

  • Zhang L, Kujawinski DM, Federherr E, Schmidt TC, Jochmann MA (2012) Caffeine in your drink: natural or synthetic? Anal Chem 84:2805–2810

    Article  CAS  Google Scholar 

  • Zhao Y, Zhang B, Chen A, Yang S, Ye Z (2014) Recent developments in application of stable isotope analysis on agro-product authenticity and traceability. Food Chem 145:300–305

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Monica Bononi.

Ethics declarations

Conflict of Interest

Monica Bononi declares that she has no conflict of interest. Giancarlo Quaglia declares that he has no conflict of interest. Fernando Tateo declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animal performed by any of the authors.

Informed Consent

Not applicable.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Bononi, M., Quaglia, G. & Tateo, F. Preliminary LC-IRMS Characterization of Italian Pure Lemon Juices and Evaluation of Commercial Juices Distributed in the Italian Market. Food Anal. Methods 9, 2824–2831 (2016). https://doi.org/10.1007/s12161-016-0479-5

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-016-0479-5

Keywords

Navigation