Analytical methods for the determination of sterigmatocystin in cheese, bread and corn products using HPLC with atmospheric pressure ionization mass spectrometric detection
1996
Scudamore, K.A. | Hetmanski, M.T. | Clarke, P.A. | Barnes, K.A. | Startin, J.R.
Methods have been developed for the determination of sterigmatocystin in bread, maize and cheese using HPLC linked to mass spectrometry (MS) atmospheric pressure chemical ionization for detection and concurrent confirmation of sterigmatocystin at levels down to less than 5 microgram/kg. Candidate extraction methods were initially checked for recovery and reproducibility by spiking commodities at a level of 200 microgram/kg of sterigmatocystin and using RPLC with post-column derivatization. Recovery was found to be greater than 90% for bread and maize, and 75% for cheese. Mass spectrometer conditions for detecting sterigmatocystin were established by injecting solutions directly into the mass spectrometer. Extracts of bread, maize grits and cheese prepared by the candidate extraction methods were examined using HPLC/MS using samples spiked at a level of 20 microgram/kg of sterigmatocystin. Results for bread and maize samples showed that the extraction procedure recovered more than 90% of added sterigmatocystin and produced extracts free of interference from co-extractives, with limits of detection of less than 2 microgram/kg for both commodities. The HPLC/MS results for cheese extracts gave lower average recoveries of 55%. These results were also more variable. However, the apparent limit of detection for sterigmatocystin in cheese was still about 4 microgram/kg.
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