关键词: amanitins mushroom toxins online liquid chromatography-diode array detector-tandem mass spectrometry (LC-DAD-MS/MS) phallotoxins wide linear range quantification wild mushrooms

Mesh : Amanita / chemistry Amanitins / analysis Chromatography, High Pressure Liquid Chromatography, Liquid Limit of Detection Mycotoxins Peptides, Cyclic Reproducibility of Results Tandem Mass Spectrometry

来  源:   DOI:10.3724/SP.J.1123.2017.02008

Abstract:
A fast and wide linear range method was established for the determination of mushroom toxins amanitins (α-amanitin,β-amanitin and γ-amanitin) and phallotoxins (phallacidin and phalloidin) in wild mushrooms by online liquid chromatography-diode array detector-tandem mass spectrometry (LC-DAD-MS/MS). The mushroom toxins were extracted with methanol, and diluted with water. The extracts were separated on an XBridgeTM BEH C18 column (150 mm×3.0 mm, 2.5 μm) under pH 10.7, measured by DAD and then analyzed by MS/MS. Basic mobile phase conditions were applied to improve the ionization efficiency of hydrogen ion adducts. The baseline separation of the analytes was obtained within 15 min. The limits of detection (LODs) of the sample matrix were 0.005-0.02 mg/kg. The toxins were quantified by the results measured by MS/MS when the toxin contents less than 2 mg/kg, and quantified by the results obtained from DAD when the contents more than 2 mg/kg. The linear range was 0.05-500 mg/kg for the whole method in one injection. The method was successfully applied to the analyses of amanitins and phallotoxins in Lepiota brunneoincarnata and white Amanita.
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