Abstract
The development of incurred reference materials containing citrinin (CIT) and their successful application in a method validation study (MVS) in order to harmonize CIT determination in food and food supplements are demonstrated. CIT-contaminated materials made of red yeast rice (RYR), wheat flour, and Ginkgo biloba leaves (GBL), as well as food supplements made of red yeast rice (FS-RYR) and Ginkgo biloba leaves (FS-GBL), were manufactured in-house via fungal cultivation on collected raw materials. The homogeneity and stability from randomly selected containers were verified according to the ISO 13528. CIT was found to be homogenously distributed and stable in all contaminated materials, with no significant degradation during the timescale of the MVS when storage was performed up to +4 °C. Next, an MVS was organized with eighteen international laboratories using the provided standard operating procedure and 12 test materials, including three RYRs (blank, <50 µg/kg, <2000 µg/kg), two wheat flours (blank, <50 µg/kg), two GBL powders (blank, <50 µg/kg), three FS-RYRs (blank, <50 µg/kg, <2000 µg/kg), and two FS-GBLs (blank, <50 µg/kg). The results of seven CIT-incurred materials showed acceptable within-laboratory precision (RSDr) varying from 6.4% to 14.6% and between-laboratory precision (RSDR) varying from 10.2% to 37.3%. Evidenced by HorRat values < 2.0, the results of the collaborative trial demonstrated that the applied analytical method could be standardized. Furthermore, the appropriateness of producing CIT reference materials is an important step towards food and feed quality control systems and the organization of proficiency tests.
Highlights
Produced by Aspergillus, Penicillium, and Monascus fungi, citrinin (CIT) is a mycotoxin that occurs often in stored grains, fruits, vegetable juices, herbs, and spices [1,2]
CIT-contaminated materials made of red yeast rice (RYR), wheat flour, and Ginkgo biloba leaves (GBL), as well as food supplements made of red yeast rice (FS-RYR) and Ginkgo biloba leaves (FS-GBL), were manufactured in-house via fungal cultivation on collected raw materials
An method validation study (MVS) was organized with eighteen international laboratories using the provided standard operating procedure and 12 test materials, including three RYRs, two wheat flours, two GBL powders, three FS-RYRs, and two Food Supplement—GBL (FS-GBL)
Summary
Produced by Aspergillus, Penicillium, and Monascus fungi, citrinin (CIT) is a mycotoxin that occurs often in stored grains, fruits, vegetable juices, herbs, and spices [1,2]. Solfrizzo et al [14] stated that there is a need for the harmonization of mycotoxin determination to ensure the verification of compliance with feed and food law and animal health and animal welfare rules In this context and within the framework of the European Regulation (EC) 882/2004 on official controls [19], the EC issued the mandate M/520 pertaining to 11 standardization priorities of analytical methods for mycotoxin determination in food [20]. The present paper describes the preparation of the incurred CIT reference materials and their use in the MVS in order to assess the inter-laboratory repeatability and reproducibility for CIT determination in food and food supplements, as requested in the standardization procedure
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