Purity Assessment of Crystalline Zearalenone

Rudolf Krska*, Elvira Welzig, Ralf D. Josephs, Wolfgang Kandler, Hans Pettersson, Susan MacDonald, Adrian Charlton, Paul Brereton, Christian Hametner, Diana Berner, Peter Zöllner

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

11 Citations (Scopus)

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.

Original languageEnglish
Pages (from-to)722-728
Number of pages7
JournalJournal of AOAC International
Volume86
Issue number4
Publication statusPublished - 01 Jul 2003
Externally publishedYes

ASJC Scopus subject areas

  • Analytical Chemistry
  • Food Science
  • Environmental Chemistry
  • Agronomy and Crop Science
  • Pharmacology

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