Skip to main content
Log in

Validation of high-performance liquid chromatography coupled with LTQ orbitrap mass spectrometry for analysis of acrylamide

  • Original Paper
  • Published:
Journal of Food Measurement and Characterization Aims and scope Submit manuscript

Abstract

Acrylamide is a food contaminant that forms through a natural chemical reaction between sugars and asparagine during high-temperature cooking processes. In this work an environmentally friendly and fast routine method for the analysis of acrylamide in Sudanese foods was successfully adapted. The method is based on sample extraction in water, purification with Carrez solutions and detection with high performance liquid chromatography–linear trap quadruple-Orbitrap-mass spectrometry (HPLC LTQ-Orbitrap MS). The performance of two analytical columns namely Kinetex C18 and Rezex ROA-organic acid was compared for acrylamide separation. The method was validated in term of linear range, limit of detection (LOD), limit of quantification (LOQ), precision (RSD%) and recovery. Good linearity (r2 > 0.9988) was achieved using standard addition method in the concentration range 0–200 µg kg− 1. The LOD is in the range from 3.24 to 4.66 µg kg− 1 and 2.47 to 3.94 µg kg− 1 for C18 and ROA columns, respectively. The precision of the method was ≤ 5.65% and 5.73% for C18 and ROA columns, respectively. Recoveries of acrylamide ranging from 86 to 98%, (n = 3) were obtained. It was successfully applied to the analysis of acrylamide in real food samples. Moreover, acrylamide precursors (free asparagine and reducing sugars) were analysed to show the relationship between their concentrations and acrylamide-forming potential.

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
Fig. 3

Similar content being viewed by others

References

  1. O. Kaplan, G. Kaya, C. Ozcan, M. Ince, M. Yaman, Acrylamide concentrations in grilled foodstuffs of Turkish kitchen by high performance liquid chromatography-mass spectrometry. Microchem. J. 93, 173–179 (2009). https://doi.org/10.1016/j.microc.2009.06.006

    Article  CAS  Google Scholar 

  2. M. Pan, K. Liu, J. Yang, L. Hong, X. Xie, S. Wang, Review of Research into the determination of Acrylamide in Foods. Foods. 9, 524 (2020). https://doi.org/10.3390/foods9040524

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  3. T. Wenzl, de la M. Calle, E. Anklam, Overview on Analytical Methods for the Determination of Acrylamide in food Products. European Commission Joint Research Centre Institute for Reference Materials and Measuremets Food Safety and Unit Retieseweg B-2440 Geel, Belgium. 2003. https://doi.org/10.1080/02652030310001605051

  4. A. Becalski, B.P.-Y. Lau, D. Lewis, S.W. Seaman, W.F. Sun, Determination of acrylamide in various food matrices. Chemistry and Safety of Acrylamide in food. Springer, 2005, 271–284

  5. F. Vezzulli, S. Triachini, A. Mulazzi, M. Lambri, T. Bertuzzi, Acrylamide: impact of precursors concentration, origin, post-harvesting process and roasting level in high quality Arabica and Robusta coffee. Int. J. Food Sci. Technol. (2022). https://doi.org/10.1111/ijfs.15900

    Article  Google Scholar 

  6. N.G. Halford, N. Muttucumaru, S.J. Powers et al., Concentrations of free amino acids and sugars in nine potato varieties: effects of storage and relationship with acrylamide formation. J. Agric. Food Chem. 60, 12044–12055 (2012). https://doi.org/10.1021/jf3037566

    Article  CAS  PubMed  Google Scholar 

  7. V. Yusà, G. Quintas, O. Pardo, P. Martí, A. Pastor, Determination of acrylamide in foods by pressurized fluid extraction and liquid chromatography-tandem mass spectrometry used for a survey of Spanish cereal-based foods. Food Addit. Contam. 23, 237–244 (2006). https://doi.org/10.1080/02652030500415678

    Article  CAS  PubMed  Google Scholar 

  8. N. Muttucumaru, S. Powers, J. Elmore, A. Briddon, D. Mottram, N. Halford, Evidence for the complex relationship between free amino acid and sugar concentrations and acrylamide-forming potential in potato. Ann. Appl. Biol. 164, 286–300 (2014). https://doi.org/10.1111/aab.12101

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  9. Z. Ciesarova, E. Kiss, E. Kolek, Study of factors affecting acrylamide levels in model systems. Czech J. food Sci. 24, 133 (2006). https://doi.org/10.17221/3308-CJFS

    Article  CAS  Google Scholar 

  10. T.M. Amrein, S. Bachmann, A. Noti et al., Potential of acrylamide formation, sugars, and free asparagine in potatoes: a comparison of cultivars and farming systems. J. Agric. Food Chem. 51, 5556–5560 (2003). https://doi.org/10.1021/jf034344v

    Article  CAS  PubMed  Google Scholar 

  11. M. Gil, P. Ruiz, J. Quijano et al., Effect of temperature on the formation of acrylamide in cocoa beans during drying treatment: an experimental and computational study. Heliyon. 6, e03312 (2020). https://doi.org/10.1016/j.heliyon.2020.e03312

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  12. T. Goldmann, A. Perisset, M.-C. Bertholet, R.H. Stadler, E.V. Petersson, K.-E. Hellenäs, Impact of extraction conditions on the content of acrylamide in model systems and food. Food Addit. Contam. 23, 437–445 (2006). https://doi.org/10.1080/02652030600632164

    Article  CAS  PubMed  Google Scholar 

  13. IARC, (1994). Acrylamide. Monographs on the evaluation of carcinogenic risks tohumans: Some industrial chemicals (Vol. 60, pp. 389–433), Lyon, France

  14. M. Negoiță, A.L. Mihai, G.A. Horneț, D.E. Duță, Development of SPE clean-up procedure for acrylamide determination from potato-based products by GC-MS/MS. Open Agric. 5, 305–316 (2020). https://doi.org/10.1515/opag-2020-0039

    Article  Google Scholar 

  15. M.M.A. Omar, W.A.W. Ibrahim, A.A. Elbashir, Sol–gel hybrid methyltrimethoxysilane–tetraethoxysilane as a new dispersive solid-phase extraction material for acrylamide determination in food with direct gas chromatography–mass spectrometry analysis. Food Chem. 158, 302–309 (2014). https://doi.org/10.1016/j.foodchem.2014.02.045

    Article  CAS  PubMed  Google Scholar 

  16. E. Tareke, P. Rydberg, P. Karlsson, S. Eriksson, M. Törnqvist, Analysis of acrylamide, a carcinogen formed in heated foodstuffs. J. Agric. Food Chem. 50, 4998–5006 (2002). https://doi.org/10.1021/jf020302f

    Article  CAS  PubMed  Google Scholar 

  17. S. Zeng, W. Chen, J. Ye, C. Yang, Investigation on the Contents of Acrylamide in Baked and Fried foods. IOP Conference Series: Earth and Environmental Science. IOP Publishing, 2020, p. 012058. https://doi.org/10.1088/1755-1315/512/1/012058

  18. L. González-Gómez, S. Morante-Zarcero, D. Pérez-Quintanilla, I. Sierra, Simultaneous determination of furanic compounds and acrylamide in insect-based foods by hplc-qqq-ms/ms employing a functionalized mesostructured silica as sorbent in solid-phase extraction. Foods. 10, 1557 (2021). https://doi.org/10.3390/foods10071557

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  19. M.M.A. Omar, A.A. Elbashir, O.J. Schmitz, Determination of acrylamide in Sudanese food by high performance liquid chromatography coupled with LTQ orbitrap mass spectrometry. Food Chem. 176, 342–349 (2015). https://doi.org/10.1016/j.foodchem.2014.12.091

    Article  CAS  PubMed  Google Scholar 

  20. S. Eslamizad, F. Kobarfard, K. Tabib, H. Yazdanpanah, J. Salamzadeh, Development of a sensitive and rapid method for determination of acrylamide in bread by LC-MS/MS and analysis of real samples in Iran IR. Iran. J. Pharm. Research: IJPR. 19, 413 (2020). https://doi.org/10.22037/ijpr.2019.111994.13474

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  21. P. Panja, Green extraction methods of food polyphenols from vegetable materials. Curr. Opin. Food Sci. 23, 173–182 (2018). https://doi.org/10.1016/j.cofs.2017.11.012

    Article  Google Scholar 

  22. K. Granby, Guidance document on analyses of acrylamide in food including analyses in the low concentration range. 2019

  23. T. Culhaoglu, D. Zheng, V. Méchin, S. Baumberger, Adaptation of the Carrez procedure for the purification of ferulic and p-coumaric acids released from lignocellulosic biomass prior to LC/MS analysis. J. Chromatogr. B 879, 3017–3022 (2011). https://doi.org/10.1016/j.jchromb.2011.08.039

    Article  CAS  Google Scholar 

  24. A.D. Troise, A. Fiore, V. Fogliano, Quantitation of acrylamide in foods by high-resolution mass spectrometry. Journal of agricultural and food chemistry. 2014; 62: 74 – 9. https://doi.org/10.1021/jf404205b J. Agric. Food Chem. 2014, 62, 74 – 79

  25. M.M.A. Omar, A.A. Elbashir, O.J. Schmitz, Capillary electrophoresis method with UV-detection for analysis of free amino acids concentrations in food. Food Chem. 214, 300–307 (2017). https://doi.org/10.1016/j.foodchem.2016.07.060

    Article  CAS  PubMed  Google Scholar 

  26. T. Delatour, A. Périsset, T. Goldmann, S. Riediker, R.H. Stadler, Improved sample preparation to determine acrylamide in difficult matrixes such as chocolate powder, cocoa, and coffee by liquid chromatography tandem mass spectroscopy. J. Agric. Food Chem. 52, 4625–4631 (2004). https://doi.org/10.1021/jf0498362

    Article  CAS  PubMed  Google Scholar 

  27. I. Gielecinska, H. Mojska, Optimisation and validation of the analytical procedure for the determination of acrylamide in coffee by LC-MS/MS with SPE clean up. Roczniki Państwowego Zakładu Higieny 2013; 64

  28. C.-L. Ky, M. Noirot, S. Hamon, Comparison of five purification methods for chlorogenic acids in green coffee beans (Coffea Sp). J. Agric. Food Chem. 45, 786–790 (1997)

    Article  CAS  Google Scholar 

  29. H.Z. Şenyuva, V. Gökmen, Study of acrylamide in coffee using an improved liquid chromatography mass spectrometry method: investigation of colour changes and acrylamide formation in coffee during roasting. Food Addit. Contam. 22, 214–220 (2005). https://doi.org/10.1080/02652030500109834

    Article  CAS  PubMed  Google Scholar 

  30. G.-A. Bent, P. Maragh, T. Dasgupta, Acrylamide in Caribbean foods–residual levels and their relation to reducing sugar and asparagine content. Food Chem. 133, 451–457 (2012). https://doi.org/10.1016/j.foodchem.2012.01.067

    Article  CAS  PubMed  Google Scholar 

  31. N. Surdyk, J. Rosén, R. Andersson, P. Åman, Effects of asparagine, fructose, and baking conditions on acrylamide content in yeast-leavened wheat bread. J. Agric. Food Chem. 52, 2047–2051 (2004). https://doi.org/10.1021/jf034999w

    Article  CAS  PubMed  Google Scholar 

  32. V. Forstova, B. Belkova, K. Riddellova, L. Vaclavik, J. Prihoda, J. Hajslova, Acrylamide formation in traditional Czech leavened wheat-rye breads and wheat rolls. Food Control. 38, 221–226 (2014). https://doi.org/10.1016/j.foodcont.2013.10.022

    Article  CAS  Google Scholar 

  33. A. Mustafa, M. Fink, A. Kamal-Eldin, J. Rosén, R. Andersson, P. Åman, Interaction effects of fermentation time and added asparagine and glycine on acrylamide content in yeast-leavened bread. Food Chem. 112, 767–774 (2009). https://doi.org/10.1016/j.foodchem.2008.05.099

    Article  CAS  Google Scholar 

  34. S. Ou, J. Shi, C. Huang et al., Effect of antioxidants on elimination and formation of acrylamide in model reaction systems. J. Hazard. Mater. 182, 863–868 (2010). https://doi.org/10.1016/j.jhazmat.2010.06.124

    Article  CAS  PubMed  Google Scholar 

  35. J. Bassama, P. Brat, P. Bohuon, R. Boulanger, Z. Günata, Study of acrylamide mitigation in model system: Effect of pure phenolic compounds. Food Chem. 123, 558–562 (2010). https://doi.org/10.1016/j.foodchem.2010.04.071

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The authors are thankful to the Deanship of Scientific Research and under the supervision of the Scientific and Engineering Research Centre at Najran University for funding this work under the Research centers Funding program grant code (NU/RCP/SERC/12/1).

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Abdalla Ahmed Elbashir.

Ethics declarations

Conflict of interest

The authors declare no conflict of interest.

Additional information

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Omar, M.M.A., Elbashir, A.A., Schmitz, O.J. et al. Validation of high-performance liquid chromatography coupled with LTQ orbitrap mass spectrometry for analysis of acrylamide. Food Measure 18, 930–939 (2024). https://doi.org/10.1007/s11694-023-02223-w

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11694-023-02223-w

Keywords

Navigation