建立了在线液相色谱-二极管阵列检测器-串联质谱技术(LC-DAD-MS/MS)同时测定野生菌中多肽类蘑菇毒素(鹅膏毒肽和鬼笔毒肽)的分析方法.样品经甲醇提取,水稀释后,在碱性条件下用XBridgeTM BEH C18柱(150 mm×3.0 mm,2.5 μm)分离,并先后用DAD和MS/MS检测.使用碱性流动相能够实现5种多肽类蘑菇毒素在15 min内达到基线分离,同时又能有效抑制质谱加钠峰[M+Na]+的响应信号,保证检测的稳定性和灵敏度.5种蘑菇毒素在0.05~500 mg/kg范围内线性关系良好,相关系数(r)>0.99;检出限为0.005~0.02 mg/kg.通过实际样品检测,证明该法操作简单、快速,灵敏度高,宽的定量检测线性范围能满足实际样品中蘑菇毒素含量变化大的特点.
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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