Abstract
In this study, the method for determining the stable carbon isotope ratio value was validated. Measurement uncertainty of stable carbon isotope ratio value of whole honey and its extracted protein derived from repeatability, reference gas, reference standards and calibration curve was calculated by applying the “bottom-up” approach according to Eurachem/CITAC guide. The expanded uncertainties for all results ranged from 0.14 to 0.19 ‰, with most of them between 0.15 and 0.16 ‰ (the coverage factor k = 2, the level of confidence p is approximately 95 %). The percentage contribution of each source to the relative combined uncertainty was calculated. The data indicated that calibration curves have more contribution to the relative combined uncertainty than repeatability and reference standards. On the other hand, the measurement uncertainty of C-4 sugar content in honey was estimated. Based on these results, 58 honey samples, such as acacia, chaste, Northeast China black bee, flowers and jujube honey, have been gathered to determine the C-4 plant sugar content adulteration in honey by elemental analyzer with an isotope ratio mass spectrometer. It can be found that all honey samples were not adulterated by C-4 plant sugar.
References
Croft LR (1987) Stable isotope mass spectrometry in honey analysis. TrAC Trends Anal Chem 6:206–209
Bogdanov S, Martin P (2002) Honey authenticity: a review. Mitt Lebensm Hyg 93:232–254
Ruoff K, Bogdanov S (2004) Authenticity of honey and other bee products. Apiacta 38:317–327
White JW (1992) 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. J AOAC Int 75:543–548
White JW, Doner LW (1978) Mass spectrometric detection of high-fructose corn syrup in honey by use of the 13C/12C ratio: collaborative study. J AOAC Int 61:746–750
Padovan GJ, De Jong D, Rodrigues LP, Marchini JS (2003) Detection of adulteration of commercial honey samples by the 13C/12C isotopic ratio. Food Chem 82:633–636
Padovan GJ, Rodrigues LP, Leme IA, De Jong D, Marchini JS (2007) Presence of C4 Sugars in honey samples detected by the carbon isotope ratio measured by IRMS. Eurasian J Anal Chem 2:134–141
White JW, Winters K (1989) Honey protein as internal standard for stable carbon isotope ratio detection of adulteration honey. J AOAC Int 72:907–911
AOAC (1999) C-4 plant sugars in honey, internal standard stable carbon isotope ratio method. AOAC Int. Gaithersburg MD (USA), 2: 27–30
AQSIQ (2002) C-4 plant sugars in honey, internal standard stable carbon isotope ratio method. AQSIQ, China, GB/T 18932.1-2002
Fisicaro P, Amarouche S, Lalere B, Labarraque G, Priel M (2008) Approaches to uncertainty evaluation based on proficiency testing schemes in chemical measurements. Accred Qual Assur 13:361–366
ISO/IEC (2009) Uncertainty of measurement—part 1: introduction to the expression of uncertainty in measurement. ISO, Geneva, Switzerland, ISO/IEC Guide 98-1:2009
Sooväli L, Rõõm E-I, Kütt A, Kaljurand I, Leito I (2006) Uncertainty sources in UV-Vis spectrophotometric measurement. Accred Qual Assur 11:246–255
Chudzinska M, Debska A, Baralkiewicz D (2012) Method validation for determination of 13 elements in honey samples by ICP-MS. Accred Qual Assur 17:65–73
Li JK, Li Y, Chen MC, Yang J, Song Y, Wang C, Jia YY, Wen AD (2013) Uncertainty evaluation for the determination of repaglinide in human plasma by LC–MS/MS. Accred Qual Assur 18:61–70
Guo BL, Wei YM, Pan JR, Li Y (2010) Stable C and N isotope ratio analysis for regional geographical traceability of cattle in China. Food Chem 118:915–920
Costinel D, Tudorache A, Ionete RE, Vremera R (2011) The impact of grape varieties to wine isotopic characterization. Anal Letters 44:2856–2864
Dehelean A, Magdas DA, Cristea G (2013) Investigation of trace metals content and carbon isotopic composition on the soil leaf-fruit chain from some Transylvanian areas. Anal Letters 46:498–507
González Martín I, Marqués Macías E, Sánchez Sánchez J, González Rivera B (1998) Detection of honey adulteration with beet sugar using stable isotope methodology. Food Chem 61:281–286
Kerkvliet JD, Meijer HAJ (2000) Adulteration of honey: relation between microscopic analysis and δ13C measurements. Apidologie 31:717–726
Cotte JF, Casabianca H, Lhéritier J, Perrucchietti C, Sanglar C, Waton H, Grenier-Loustalot MF (2007) 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. Anal Chim Acta 582:125–136
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 and liquid chromatography—isotope ratio mass spectrometry (δ13C-EA/LC-IRMS). Apidologie 39:574–587
Simsek A, Bilsel M, Goren AC (2012) 13C/12C pattern of honey from Turkey and determination of adulteration in commercially available honey samples using EA-IRMS. Food Chem 130:1115–1121
Schellenberg A, Chmielus S, Schlicht C, Camin F, Perini M, Bontempo L, Heinrich K, Kelly SD, Rossmann A, Thomas F, Jamin E, Horacek M (2010) Multielement stable isotope ratios (H, C, N, S) of honey from different European regions. Food Chem 121:770–777
Kropf U, Golob T, Nečemer M, Kump P, Korošec M, Bertoncelj J, Ogrinc N (2010) Carbon and nitrogen natural stable isotopes in Slovene honey: adulteration and botanical and geographical aspects. J Agric Food Chem 58:12794–12803
Eurachem/CITAC (2012) Quantifying uncertainty in analytical measurement (QUAM: 2012), 3rd edn. http://www.eurachem.org/index.php/publications/guides/quam
Hässelbarth W (1998) Measurement uncertainty procedures revisited: direct determination of uncertainty and bias handling. Accred Qual Assur 3:418–422
Yenisoy-Karakaş S (2012) Estimation of uncertainties of the method to determine the concentrations of Cd, Cu, Fe, Pb, Sn and Zn in tomato paste samples analysed by high resolution ICP-MS. Food Chem 132:1555–1561
Acknowledgments
This study was financially supported by the Science and Technology Plan Project of General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China (2013IK200).
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Chen, H., Fan, Cl., Wang, Zb. et al. Evaluation of measurement uncertainty in EA–IRMS: for determination of δ 13C value and C-4 plant sugar content in adulterated honey. Accred Qual Assur 18, 351–358 (2013). https://doi.org/10.1007/s00769-013-0990-y
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00769-013-0990-y