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J Agric Food Chem. 2013 May 22;61(20):4822-30. doi: 10.1021/jf401139u. Epub 2013 May 9.

Determination of multiple mycotoxins in dietary supplements containing green coffee bean extracts using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).

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1
Center for Food Safety and Applied Nutrition, Office of Regulatory Science, U.S. Food and Drug Administration, 5100 Paint Branch Parkway, HFS-717, College Park, MD 20740, USA. Lukas.Vaclavik@fda.hhs.gov

Abstract

An ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the determination of 34 mycotoxins in dietary supplements containing green coffee bean (GCB) extracts was developed, evaluated, and used in the analysis of 50 commercial products. A QuEChERS-like procedure was used for isolation of target analytes from the examined matrices. Average recoveries of the analytes were in the range of 75-110%. The precision of the method expressed as relative standard deviation was below 12%. Limits of detection (LODs) and limits of quantitation (LOQs) ranged from 1.0 to 50.0 μg/kg and from 2.5 to 100 μg/kg, respectively. Due to matrix effects, the method of standard additions was used to ensure accurate quantitation. Ochratoxin A, ochratoxin B, fumonisin B1 and mycophenolic acid were found in 36%, 32%, 10%, and 16% of tested products, respectively. Mycotoxins occurred in the following concentration ranges: ochratoxin A, <1.0-136.9 μg/kg; ochratoxin B, <1.0-20.2 μg/kg; fumonisin B1, <50.0-415.0 μg/kg; mycophenolic acid, <5.0-395.0 μg/kg. High-resolution mass spectrometry operated in full MS and MS/MS mode was used to confirm the identities of the reported compounds.

PMID:
23631685
DOI:
10.1021/jf401139u
[Indexed for MEDLINE]
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