Development of a certified reference material for the accurate determination of type B trichothecenes in corn.

ABSTRACT

A corn flour certified reference material (KRISS CRM 108-01-011) was developed to ensure accurate and reliable measurements of type B trichothecenes (deoxynivalenol, nivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol), and deoxynivalenol-3-glucoside. The material was freeze-dried, ground, sieved, and well-mixed. The final produced CRM was packaged at 14 g per unit and stored at -70 °C. The certification was performed using isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). For simultaneous characterization and homogeneity assessments, ten units were randomly selected and analyzed. The among-unit relative standard deviations were below 1 % for all mycotoxins, indicating excellent homogeneity of the CRM. The stability of the CRM was also assessed at various designated temperatures and test periods. The uncertainties of the certified values varied between 2.4 % and 6.2 %, thereby confirming their higher-order metrological quality to provide references for testing laboratories. In case of deoxynivalenol-3-glucoside, an information value was assigned due to the lack of its traceability to the SI units.