The present interlaboratory comparison study involved nine laboratories located throughout the world that tested for 24 regulated and non-regulated mycotoxins by applying their in-house LC-MS/MS multi-toxin method to 10 individual lots of 4 matrix commodities, including complex chicken and swine feed, soy and corn gluten. In total, more than 6000 data points were collected and analyzed statistically by calculating a consensus value in combination with a target standard deviation following a modified Horwitz equation. The performance of each participant was evaluated by a z-score assessment with a satisfying range of ±2, leading to an overall success rate of 70% for all tested compounds. Equal performance for both regulated and emerging mycotoxins indicates that participating routine laboratories have successfully expanded their analytical portfolio in view of potentially new regulations. In addition, the study design proved to be fit for the purpose of providing future certified reference materials, which surpass current analyte matrix combinations and exceed the typical scope of the regulatory framework.

Department of Agrobiotechnology Institute of Bioanalytics and Agro Metabolomics University of Natural Resources and Life Sciences 3430 Vienna Austria

Department of Food Analysis and Nutrition University of Chemistry and Technology Prague Technicka 3 16628 Prague 6 Czech Republic

Department of Food Chemistry and Toxicology Faculty of Chemistry University of Vienna Währinger Straße 38 40 1090 Vienna Austria

Department of Pharmacology and Toxicology National Veterinary Research Institute 24 100 Pulawy Poland

FFoQSI Austrian Competence Centre for Feed and Food Quality Safety and Innovation FFoQSI GmbH 3430 Tulln Austria

Institute for Global Food Security Queens University Belfast Belfast BT7 1NN UK

Key Laboratory of Industrial Biotechnology Ministry of Education School of Biotechnology Jiangnan University Wuxi 214101 China

LVA GmbH Department for Residue Analysis Magdeburggasse 10 3400 Klosterneuburg Austria

Romer Labs Analytical Service Ltd No 6 1 Chunyu Road Wuxi 214000 China

Romer Labs Diagnostic GmbH Analytical Service Department Technopark 5 3430 Tulln Austria

Romer Labs Division Holding GmbH Marketing Department Erber Campus 1 3131 Getzersdorf Austria

Romer Labs Division Holding GmbH Technical Support Department Technopark 5 3430 Tulln Austria

Romer Labs US Inc Analytical Service Department 1301 Stylemaster Drive Union MO 63084 USA

Zobrazit více v PubMed

Eskola M., Elliott C.T., Hajšlová J., Steiner D., Krska R. Towards a dietary-exposome assessment of chemicals in food: An update on the chronic health risks for the European consumer. Crit. Rev. Food Sci. Nutr. 2020;60:1890–1911. doi: 10.1080/10408398.2019.1612320. PubMed DOI

Eskola M., Kos G., Elliott C.T., Hajšlová J., Mayar S., Krska R. Worldwide contamination of food-crops with mycotoxins: Validity of the widely cited ‘FAO estimate’ of 25% Crit. Rev. Food Sci. Nutr. 2020;60:2773–2789. doi: 10.1080/10408398.2019.1658570. PubMed DOI

De Girolamo A., Ciasca B., Stroka J., Bratinova S., Pascale M., Visconti A., Lattanzio V.M.T. Performance evaluation of LC–MS/MS methods for multi-mycotoxin determination in maize and wheat by means of international Proficiency Testing. TrAC Trends Anal. Chem. 2017;86:222–234. doi: 10.1016/j.trac.2016.11.005. DOI

Malachová A., Sulyok M., Beltrán E., Berthiller F., Krska R. Optimization and validation of a quantitative liquid chromatography-tandem mass spectrometric method covering 295 bacterial and fungal metabolites including all regulated mycotoxins in four model food matrices. J. Chromatogr. A. 2014;1362:145–156. doi: 10.1016/j.chroma.2014.08.037. PubMed DOI

Krska R., Schubert-Ullrich P., Molinelli A., Sulyok M., Macdonald S., Crews C. Mycotoxin analysis: An update. Food Addit. Contam. Part A Chem. Anal. Control Expo. Risk Assess. 2008;25:152–163. doi: 10.1080/02652030701765723. PubMed DOI

FAO . Climate Change: Unpacking the Burden on Food Safety. FAO; Rome, Italy: 2020.

Steiner D., Malachová A., Sulyok M., Krska R. Challenges and future directions in LC-MS-based multiclass method development for the quantification of food contaminants. Anal. Bioanal. Chem. 2021;413:25–34. doi: 10.1007/s00216-020-03015-7. PubMed DOI PMC

Steiner D., Sulyok M., Malachová A., Mueller A., Krska R. Realizing the simultaneous liquid chromatography-tandem mass spectrometry based quantification of >1200 biotoxins, pesticides and veterinary drugs in complex feed. J. Chromatogr. A. 2020;1629:461502. doi: 10.1016/j.chroma.2020.461502. PubMed DOI

Tittlemier S.A., Cramer B., Dall’Asta C., DeRosa M.C., Lattanzio V.M.T., Malone R., Maragos C., Stranska M., Sumarah M. Developments in mycotoxin analysis: An update for 2020–2021. World Mycotoxin J. 2022;15:3–25. doi: 10.3920/WMJ2021.2752. DOI

Steiner D., Krska R., Malachová A., Taschl I., Sulyok M. Evaluation of Matrix Effects and Extraction Efficiencies of LC-MS/MS Methods as the Essential Part for Proper Validation of Multiclass Contaminants in Complex Feed. J. Agric. Food Chem. 2020;68:3868–3880. doi: 10.1021/acs.jafc.9b07706. PubMed DOI PMC

Sulyok M., Stadler D., Steiner D., Krska R. Validation of an LC-MS/MS-based dilute-and-shoot approach for the quantification of >500 mycotoxins and other secondary metabolites in food crops: Challenges and solutions. Anal. Bioanal. Chem. 2020;412:2607–2620. doi: 10.1007/s00216-020-02489-9. PubMed DOI PMC

General Requirements for the Competence of Testing and Calibration Laboratories. Vol. 2005 International Standard Organization; Geneva, Switzerland: 2005.

Sibanda L., McCallum K., Plotan M., Webb S., Snodgras B., Muenks Q., Porter J., Fitzgerald P. Interlaboratory collaboration to determine the performance of the Randox food diagnostics biochip array technology for the simultaneous quantitative detection of seven mycotoxins in feed. World Mycotoxin J. 2022;15:241–250. doi: 10.3920/WMJ2021.2696. DOI

Statistical methods for use in proficiency testing by interlaboratory comparison. International Standard Organization; Geneva, Switzerland: 2015. p. 207.

Commission of the European Union. COMMISSION REGULATION (EC) No 1881/2006. Off. J. Eur. Union. 2006;364:15–24.

Thompson M., Ellison S.L.R., Wood R. The International Harmonized Protocol for the proficiency testing of analytical chemistry laboratories (IUPAC Technical Report) Pure Appl. Chem. 2006;78:145–196. doi: 10.1351/pac200678010145. DOI

Asuero A.G., Sayago A., Gonzalez A.G. The correlation coefficient: An overview. Crit. Rev. Anal. Chem. 2006;36:41–59. doi: 10.1080/10408340500526766. DOI

Häggblom P., Nordkvist E. Deoxynivalenol, zearalenone, and Fusarium graminearum contamination of cereal straw; field distribution; and sampling of big bales. Mycotoxin Res. 2015;31:101–107. doi: 10.1007/s12550-015-0220-z. PubMed DOI PMC

Rheeder J.P., Marasas W.F.O., Vismer H.F. Production of fumonisin analogs by Fusarium species. Appl. Environ. Microbiol. 2002;68:2101–2105. doi: 10.1128/AEM.68.5.2101-2105.2002. PubMed DOI PMC

Jestoi M. Emerging fusarium-mycotoxins fusaproliferin, beauvericin, enniatins, and moniliformin—A review. Crit. Rev. Food Sci. Nutr. 2008;48:21–49. doi: 10.1080/10408390601062021. PubMed DOI

Ropejko K., Twarużek M. Zearalenone and Its Metabolites-General Overview, Occurrence, and Toxicity. Toxins. 2021;13:35. doi: 10.3390/toxins13010035. PubMed DOI PMC

Streit E., Schwab C., Sulyok M., Naehrer K., Krska R., Schatzmayr G. Multi-mycotoxin screening reveals the occurrence of 139 different secondary metabolites in feed and feed ingredients. Toxins. 2013;5:504–523. doi: 10.3390/toxins5030504. PubMed DOI PMC

Gruber-Dorninger C., Novak B., Nagl V., Berthiller F. Emerging Mycotoxins: Beyond Traditionally Determined Food Contaminants. J. Agric. Food Chem. 2017;65:7052–7070. doi: 10.1021/acs.jafc.6b03413. PubMed DOI

Martínez-Domínguez G., Romero-González R., Arrebola F.J., Garrido Frenich A. Multi-class determination of pesticides and mycotoxins in isoflavones supplements obtained from soy by liquid chromatography coupled to Orbitrap high resolution mass spectrometry. Food Control. 2016;59:218–224. doi: 10.1016/j.foodcont.2015.05.033. PubMed DOI

Habinshuti I., Chen X., Yu J., Mukeshimana O., Duhoranimana E., Karangwa E., Muhoza B., Zhang M., Xia S., Zhang X. Antimicrobial, antioxidant and sensory properties of Maillard reaction products (MRPs) derived from sunflower, soybean and corn meal hydrolysates. LWT. 2019;101:694–702. doi: 10.1016/j.lwt.2018.11.083. DOI

Patil U.S., King S., Holleran S., White K., Stephenson C., Reuther J. Identifying challenges and risks associated with the analysis of major mycotoxins in feed and botanicals. J. AOAC Int. 2019;102:1689–1694. doi: 10.5740/jaoacint.19-0105. PubMed DOI

Rao Z.-X., Tokach M.D., Woodworth J.C., DeRouchey J.M., Goodband R.D., Calderón H.I., Dritz S.S. Effects of fumonisin-contaminated corn on growth performance of 9 to 28 kg nursery pigs. Toxins. 2020;12:604. doi: 10.3390/toxins12090604. PubMed DOI PMC

Kovalsky P., Kos G., Nährer K., Schwab C., Jenkins T., Schatzmayr G., Sulyok M., Krska R. Co-occurrence of regulated, masked and emerging mycotoxins and secondary metabolites in finished feed and maize–An extensive survey. Toxins. 2016;8:363. doi: 10.3390/toxins8120363. PubMed DOI PMC

Vohra M., Manwar J., Manmode R., Padgilwar S., Patil S. Bioethanol production: Feedstock and current technologies. J. Environ. Chem. Eng. 2014;2:573–584. doi: 10.1016/j.jece.2013.10.013. DOI

Saunders D.S., Meredith F.I., Voss K.A. Control of Fumonisin: Effects of Processing. Environ. Health Perspect. 2001;109:333–336. doi: 10.2307/3435027. PubMed DOI PMC

Prettl Z.S., Lepossa A., Tóth É., Kelemen-Horváth I., Németh Á.S., Nagy E. Effects and changes of zearalenone and fumonisin contamination in corn-based bioethanol process. Hung. J. Ind. Chem. 2011;39:427–431.

Berwanger E., Nunes R.V., Pasquetti T.J., Murakami A.E., De Oliveira T.M.M., Bayerle D.F., Frank R. Sunflower cake with or without enzymatic complex for broiler chickens feeding. Asian-Australasian J. Anim. Sci. 2017;30:410–416. doi: 10.5713/ajas.15.0644. PubMed DOI PMC

Varga E., Glauner T., Köppen R., Mayer K., Sulyok M., Schuhmacher R., Krska R., Berthiller F. Stable isotope dilution assay for the accurate determination of mycotoxins in maize by UHPLC-MS/MS. Anal. Bioanal. Chem. 2012;402:2675–2686. doi: 10.1007/s00216-012-5757-5. PubMed DOI PMC

Wang J., Cheung W. Determination of pesticides in soy-based infant formula using liquid chromatography with electrospray ionization tandem mass spectrometry. J. AOAC Int. 2006;89:214–224. doi: 10.1093/jaoac/89.1.214. PubMed DOI

Meneely J.P., Ricci F., Van Egmond H.P., Elliott C.T. Current methods of analysis for the determination of trichothecene mycotoxins in food. TrAC Trends Anal. Chem. 2011;30:192–203. doi: 10.1016/j.trac.2010.06.012. DOI

Guide 35—Reference Materials—Guidance for Characterization and Assessment of Homogeneity and Stability. Vol. 8. International Standard Organization; Geneva, Switzerland: 2017. p. 114.

Linsinger T.P.J., Pauwels J., Van Der Veen A.M.H., Schimmel H., Lamberty A. Homogeneity and stability of reference materials. Accredit. Qual. Assur. 2001;6:20–25. doi: 10.1007/s007690000261. DOI

Analytical Quality Control and Method Validation for Pesticide Residues Analysis in Food and Feed. European Commission; Brussels, Belgium: 2021.

Bao L., Bao Z., Zhang Y., Liang C., Lu N., Liu X., Jin Y., Pei J.Z., Ge M., Tian L. Aflatoxin Testing in Peanuts: A Proficiency Assessment Scheme for Chinese Analytic Laboratories. Food Chem. Contam. 2009;92:481–486. doi: 10.1093/jaoac/92.2.481. PubMed DOI

Thompson M. Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in relation to fitness for purpose criteria in proficiency testing. Anal. Commun. 2000;125:385–386. doi: 10.1039/b000282h. DOI