【摘要】 [目的]建立一种基于超高效液相色谱-串联质谱法(UPLC-MS/MS)快速测定野生毒蕈中6种鹅膏毒肽和鬼笔毒肽类毒素的分析方法。[方法]将采集的四川野生毒蕈子实体低温烘干,用甲醇超声提取,40℃旋转蒸发近干,加水复溶,Oasis HLB固相萃取小柱净化,经Waters HSS T3色谱柱分离,ESI正离子模式下多反应监测(MRM)方式分析。[结果]6种毒肽在50～1 000μg/kg具有良好的线性关系,相关系数均大于0.99,方法检出限为30μg/kg。α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、二羟鬼笔毒肽、羧基二羟鬼笔毒肽、羧基三羟鬼笔毒肽在低、中、高3个浓度的平均回收率在93.1%～117.5%,变异系数(CV)在1.49%～7.77%。[结论]该方法能准确、灵敏地测定野生毒蕈中6种毒肽,适用于野生菌中毒肽毒素的测定。更多还原

【Abstract】 [Objective]To establish a method for rapid determination of 6 kinds of amanitins and phallotoxins in wild poisonous mushrooms by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).[Method]The wild mushrooms samples collected in Sichuan were dried at low temperature, the amanitins and phallotoxins in samples were extracted with methanol by ultrasonic extraction, then 40 ℃ rotary evaporation drying,water redissolution, purified by HLB solid phase extraction column and separated on Waters HSS T3 column, lastly detected by electrospray(ESI+) in MRM mode. [Result] The 6 kinds of amanitins and phallotoxins had good linear relationships in the range of concentration 50-1000 μg/kg with the correlation coefficient value greater than 0.99.The detection limits of 6 kinds of amanitins and phallotoxins were 30 μg/kg.The average recovery rates of α-amanitin, β-amanitin, γ-amanitin, phalloidin, phallacidin and phallisacin at 3 spiked levels were 93.1%-117.5%. The coefficients of variation were 1.49%-7.77%. [Conclusion]The method can accurately and sensitively determine 6 kinds of amanitins and phallotoxins in poisonous mushrooms, which is suitable for the detection of amanitins and phallotoxins in wild mushrooms.更多还原