European Food Research and Technology

, Volume 245, Issue 10, pp 2331–2341 | Cite as

Innovative techniques for identifying a mechanically separated meat: sample irradiation coupled to electronic spin resonance

  • Michele Tomaiuolo
  • Antonio Eugenio Chiaravalle
  • Michele Mangiacotti
  • Antonio Petrella
  • Aurelia Di Taranto
  • Marco IammarinoEmail author
Original Paper


As reported by European Food Safety Authority, the identification of a meat product obtained from mechanically separated meat (MSM) has significance from a point of view both of food quality and safety. As a consequence, it recommended the development of innovative methods for identifying a MSM. The electron spin resonance (ESR) spectroscopy is a useful tool for identifying previously irradiated meat products containing bone. Due to the presence of bone fragments and periosteum (bone skin) in MSM, this technique was exploited for developing an innovative analytical method for identifying a MSM and quantifying bone fragments. This procedure is based on sample irradiation at 1 kGy, after proper sample pre-treatment, followed by analysis by ESR spectroscopy. This analytical method was validated following a validation protocol developed “in-house”. The presence of bone fragments, due to MSM addition in the product formulation, lead to the identification of six characteristic signals on the ESR spectrum. Among these, three signals were always verified in all commercial samples analysed (wurstel), composed of different percentages of MSM. The quantitative determination of bone fragments was also studied through method validation. Good analytical performances were obtained in terms of selectivity, with no interfering signals; sensitivity, with LOD and LOQ equal to 16 and 48 mg/100 g (w/w f.w.), respectively; accuracy, as mean CV % = 12.8% and mean error % = 9%; (n = 18), ruggedness (method applicable to different types of meat products), and measurement uncertainty of 14.6%, confirming that the procedure can be developed successfully for accurate qualitative–quantitative analysis.


Mechanically separated meat Food irradiation Electronic spin resonance Meat quality Food safety Validation 



This work was supported by the Italian Ministry of Health who funded the Project code GR-2013-02358862. Ms. Mariagrazia Russo and Mr. Michele Nicolini (Istituto Zooprofilattico Sperimentale della Puglia e della Basilicata, Foggia, Italy) are gratefully acknowledged for technical assistance.


This work was funded by the Italian Ministry of Health (Grant number GR-2013-02358862).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Compliance with ethics requirements

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


  1. 1.
    World Health Organization/Food and Agriculture Organization (2002) Joint WHO/FAO expert consultation on diet, nutrition and the prevention of chronic diseases. Accessed 13 Jul 2018
  2. 2.
    World Health Organization/International Agency for Research on Cancer (2015) IARC Monographs evaluate consumption of red meat and processed meat. Accessed 13 Jul 2018
  3. 3.
    Iammarino M, Marino R, Albenzio M (2017) How meaty? Detection and quantification of adulterants, foreign proteins and food additives in meat products. Int J Food Sci Tech 52(4):851–863CrossRefGoogle Scholar
  4. 4.
    Food and Agriculture Organization FAO (2003) World agriculture: towards 2015/2030—an FAO perspective. Accessed 13 Jul 2018
  5. 5.
    Commission European (2004) Regulation (EC) No 853/2004 of the European Parliament and of the Council of 29 April 2004 laying down specific hygiene rules for on the hygiene of foodstuffs. Off J Eur Union L 139:55Google Scholar
  6. 6.
    European Food Safety Authority (2013) Scientific Opinion on the public health risks related to mechanically separated meat (MSM) derived from poultry and swine. EFSA J 11(3):3137CrossRefGoogle Scholar
  7. 7.
    Commission European (2001) Regulation (EC) No 999/2001 of the European Parliament and of the Councilof 22 May 2001 laying down rules for the prevention, control and eradication of certain transmissible spongiform encephalopathies. Off J Eur Union L 147:5Google Scholar
  8. 8.
    Branscheid W, Judash M, Höreth R (2009) The morphological detection of bone and cartilage particles inmechanically separated meat. Meat Sci 81:46–50CrossRefGoogle Scholar
  9. 9.
    Tremlová B, Štarha P (2003) Histological analysis of different kinds of mechanically recovered meat. Archiv fur Lebensmittelhygiene 57:85–91Google Scholar
  10. 10.
    Stenzel WR, Hildebrandt G (2006) Analytical criteria for the detection of mechanically separated meat (MSM). Results of a survey of the calcium content in minced meat. Fleischwirtschaft 86:96–98Google Scholar
  11. 11.
    European Committee for Standardization (1996) EN 1786—Detection of irradiated food containing bone—method by ESR spectroscopy. Accessed 18 Jul 2018
  12. 12.
    Commission European (2013) Regulation (EC) No 53/2013 of 16 January 2013 amending Regulation (EC) No 152/2009 as regards the methods of analysis for the determination of constituents of animal origin for the official control of feed. Off J Eur Union L20:33–43Google Scholar
  13. 13.
    United States Department of Agriculture (2018) Moisture determination-CLG-MOI.04 Rev.04. USDA Food Safety and Inspection Service, Office of Public Health Science. Accessed 22 Jul 2018
  14. 14.
    Randall EL (1974) Improved method for fat and oil analysis by a new process of extraction. J Assoc Off Ana Chem 57:1165–1168Google Scholar
  15. 15.
    Association of Official Analytical Chemists (2006) AOAC Official Method 2003.06—Randall/Soxtec/Hexanes Extraction-Submersion Method. Official Methods of Analysis of AOAC INTERNATIONAL, 20th EditionGoogle Scholar
  16. 16.
    Iammarino M, dell’Oro D, Bortone N, Mangiacotti M, Chiaravalle AE (2016) Optimisation and validation of a multi-matrix ultrasensible radiochemical method for the determination of radiostrontium in solid foodstuffs by liquid scintillation counting. Food Anal Method 9:95–104CrossRefGoogle Scholar
  17. 17.
    Commission European (2002) Decision (EC) No. 657/2002 of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off J Eur Union L221:8–36Google Scholar
  18. 18.
    European Parliament/Council of the European Union (2017) Regulation (EU) 2017/625 of the European Parliament and of the Council of 15 March 2017. Off J Eur Union L95:1–142Google Scholar
  19. 19.
    Thompson M, Ellison SRL, Wood R (2002) Harmonized guidelines for single laboratory validation of methods of analysis. Pure Appl Chem 74(5):835–855CrossRefGoogle Scholar
  20. 20.
    Nagy J, Lenhardt L, Korimová L, Dičáková Z, Popelka P, Pipová M, Tomková I (2007) Comparison of the quality of mechanically deboned poultry meat after different methods of separation. Meso 9:92–95Google Scholar
  21. 21.
    Grunden LP, Macneil JH (1973) Examination of bone content in mechanically deboned poultry meat by EDTA and atomic absorption spectrophotometric methods. J Food Sci 38(4):712–713CrossRefGoogle Scholar
  22. 22.
    Miller EJC, Miller JN (1993) Statistics for analytical chemistry, 3rd edn. Ellis Horwood PTR Prentice Hall, New YorkGoogle Scholar
  23. 23.
    Youden WJ, Steiner EH (1975) Statistical manual of the AOAC. Association of the Official Analytical Chemists, Washington DCGoogle Scholar
  24. 24.
    Hund E, Massart DL, Smeyers-Verbeke J (2001) Operational definitions of uncertainty. TrAC Trends Anal Chem 20(8):394–406CrossRefGoogle Scholar
  25. 25.
    Cammack R, Cooper CE (1993) Electron paramagnetic resonance spectroscopy of iron complexes and iron-containing proteins. Method Enzymol 227:353–384CrossRefGoogle Scholar
  26. 26.
    Cammack R, Shergill JK (1996) EPR spectroscopy of proteins. In: Price NC (ed) Proteins Labfax. Bios Scientific Publishers, OxfordGoogle Scholar
  27. 27.
    Park YD, Kim DY, Jin CH, Yang HS, Choi DS, Yook H-S, Byun M-W, Jeong IY (2011) Development of a method based on ESR spectroscopy for the identification of irradiated beef, pork, and chicken meats. Food Sci Biotechnol 20(2):367–370CrossRefGoogle Scholar
  28. 28.
    Goto M, Tanabe H, Miyahara M (2000) Detection of irradiated chicken by hydrocarbon method and ESR method. Shokuhin Shosha 35(1–2):23–34Google Scholar
  29. 29.
    Duarte CL, Villavicencio ALCH, Del Mastro LN, Wiendl FM (1995) Detection of irradiated chicken by ESR spectroscopy of bone. Radiat Phys Chem 46(4–6):689–692 (Part 1) CrossRefGoogle Scholar
  30. 30.
    Dalipi R, Berneri R, Curatolo M, Borgese L, Depero LE, Sangiorgi E (2018) Total reflection X-ray fluorescence used to distinguish mechanically separated from non-mechanically separated meat. Spectrochim Acta B 148:16–22CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.National Reference Center for the Detection of Radioactivity in Feed and FoodstuffIstituto Zooprofilattico Sperimentale della Puglia e della BasilicataFoggiaItaly
  2. 2.Chemistry DepartmentIstituto Zooprofilattico Sperimentale della Puglia e della BasilicataFoggiaItaly
  3. 3.Diagnostics Operational UnitIstituto Zooprofilattico Sperimentale della Puglia e della BasilicataFoggiaItaly

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