title: Determination of multiple mycotoxins in dietary supplements containing green coffee bean extracts using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).
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.
authors: 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
authors: Lukas
authors: L
authors: Vaclavik
authors: Marta
authors: M
authors: Vaclavikova
authors: Timothy H
authors: TH
authors: Begley
authors: Alexander J
authors: AJ
authors: Krynitsky
authors: Jeanne I
authors: JI
authors: Rader
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D040503:Coffea / Q000737:chemistry*; D019587:Dietary Supplements / Q000032:analysis*; D037341:Fumonisins / Q000032:analysis; D057230:Limit of Detection; D009173:Mycophenolic Acid / Q000032:analysis; D009183:Mycotoxins / Q000032:analysis*; D009793:Ochratoxins / Q000032:analysis; D010936:Plant Extracts / Q000737:chemistry*; D012639:Seeds / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D037341:Fumonisins; D009183:Mycotoxins; D009793:Ochratoxins; D010936:Plant Extracts; C025589:ochratoxin A; C056933:fumonisin B1; C045354:ochratoxin B; D009173:Mycophenolic Acid