In an inter laboratory study of the AOAC/lnternational Union of Pure and Applied Chemistry (IUPAC)/ Nordic Committee on Food Analysis (NMKL) liquid chromatographic method for ochratoxin A (OTA), 3 spiked samples each of wheat bran and rye and 3 naturally contaminated barley samples with expected OTA contents between 2 and 9 μg/kg were analyzed by 12 European laboratories. Mean recoveries ranged from 64 to 72%. Within-laboratory standard deviations were 21,17, and 12% for wheat bran, rye, and barley, respectively. Corresponding between-laboratory standard deviations were 23-28,20-28, and 18-31%. Horwitz ratio values ranged from 0.50 to 0.77. The method was accepted as an official NMKL method for determining OTA at ≥2 μg/kg in cereals and cereal products.
Several previous interlaboratory studies in the field of mycotoxin analysis have revealed considerable problems, apparent as high between-laboratory standard deviations, or rather non-comparable and non-traceable results. A major reason is lack of proper calibrants for external calibration. Public awareness of substances that mimic or interfere with the activity of natural hormones (endocrine disrupters) has led to increased interest in mycotoxins with estrogenic potential, e.g. zearalenone (ZON). During a large-scale standard measurement and testing (SMT) project of the European Commission (EC) dealing with the preparation and certification of reference materials for determination of the mycotoxin ZON in maize, a ZON calibrant in acetonitrile was prepared and intensively checked for purity, homogeneity, and stability. Preparation of the material, study of its homogeneity and stability, and characterisation of the calibrant on the basis of its preparation, with discussion of the results obtained, are described in this paper. The certified value of 9.95 micro g mL(-1) for ZON in acetonitrile and its corresponding expanded uncertainty of +/-0.30 micro g mL(-1) were calculated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM).
No abstract
Commercially available solid zearalenone (ZON) to be used as a certified liquid calibrant (BCR-699) in a project funded by the European Commission within the Standard Measurement and Testing program was characterized and its purity determined. The degree of purity of the ZON was examined by UV spectrophotometer, liquid chromatography (LC) with diode array and fluorescence detection, 1H and 13C-NMR spectrometry, LC–mass spectrometry (LC/MS/MS), ion chromatography (IC), and differential scanning calorimetry (DSC). The diagrams obtained from DSC analysis and the UV spectrum showed no detectable impurities. Likewise, no impurities were observed by LC analysis with both diode array and fluorescence detection. IC determination revealed negligible contamination of ZON with chloride of 0.020 ± 0.005% and nitrate of 0.016 ± 0.006%. Zearalanone (ZAN) was identified as one of 2 minor (0.2%) impurities by LC/MS/MS. The 1H-NMR measurements revealed an additional peak, which has not been previously reported in the literature. It could be identified as part of the ZON spectrum as the signal arising from the phenolic proton attached to C4'. The manufacturer states an additional contamination with 0.2% methylene chloride, which could be confirmed to an extent of 0.1% by 1H-NMR. Minor impurities, whose structures remain unknown, were discovered at 3.5 and <1 ppm. Total percentage of impurities based on NMR measurement was estimated not to exceed 1%. A purity of 99.5% with a tolerance of ±0.5% was finally attributed to the ZON studied in this project.
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