CCQM Key Comparison track A CCQM-K168: Non-polar analytes in high carbohydrate food matrix: trans-zearalenone in maize powder
Authors: Li X Q , Li H M , Jiao H , Guo Z H , Zhang Q H , Kneeteman L E , Lewin M , Rego E C Pires do , Leal R V , Violante F G M , Monteiro T M , Garrido B C , Melanson J , Chan P K , Fung, W H , Ng, CS , Yip Y C , Barrios J , Salinas A , Giraldo J , Koch M , Riedel J , Polzer J , Borzekowski A , Rausch A K , Giannikopoulou P , Skotidaki I , Kakoulides E , Nakamura K , Choi K , Krylov A , Mikheeva A , Teo T L , Cheow P S , Lu T , Tong B , Claasen D , Prevoo-Franzsen, D , Fernandes-Whaley M , Marbumrung S , Boonyakong C , Bilsel M , Gokcen T , Ozen S A 
Published: October 2023

Main text
Demonstrating competency and equivalence for the measurement capacity of contaminants and nutrients in primary foodstuffs is a priority of the OAWG 10-year strategy for Track A core comparisons. Such measurements have posed significant challenges for reference material producers and calibration service providers. This key comparison (KC), under the topic of "non- polar analyte in high carbohydrate food matrix: trans-Zearalenone (trans-ZEN) in maize powder", was a sector of the model system selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to demonstrate the Calibration and Measurement Capabilities (CMCs) of National Metrology Institutes (NMIs) and Designated Institutes (DIs).
17 NMIs and DIs participated in the Track A KC CCQM-K168 "non-polar analyte in high carbohydrate food matrix: trans-ZEN in maize powder". Participants were requested to evaluate the mass fraction (μg/kg) of trans-ZEN in maize powder material. Methods like liquid-liquid extraction and SPE were applied in the pre-treatment, and HPLC-MS/MS and HPLC-FLD were used for detection by the participants. The mass fractions for trans-ZEN were in the range of (91.8 to 169) μg/kg with standard uncertainties of (1.5 to 24.7) μg/kg, and corresponding relative standard uncertainties from 1.5% to 14.6%. Two laboratories, INTI and BAM were excluded from the key comparison reference value (KCRV) evaluation. INTI result was identified as an outlier and confirmed their method had insufficient specificity. For BAM the calibration approach they used does not meet the CIPM traceability requirements. The other 15 laboratories included in the calculation of the consensus KCRV all agreed within their standard uncertainties. Hierarchical Bayes was used as estimators in calculating KCRV and standard uncertainty.
Successful participation in CCQM-K168 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 1 μg/kg to 1000 μg/kg in a high carbohydrate food matrix.
To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.
The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).