超高效液相色谱-串联质谱法测定毒蘑菇中5种强毒性蘑菇毒素含量

Determination of 5 kinds of virulent mushroom toxins in poisonous mushroom by ultra performance liquid chromatography tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法快速检测毒蘑菇中α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、羧基二羟鬼笔毒肽和二羟鬼笔毒肽5种强毒性蘑菇毒素含量的分析方法。方法样品经甲醇/水(3:7, V:V)混合液超声提取,离心后取上清液过0.22μm微孔滤膜,C18色谱柱分离,超高效液相色谱-串联质谱仪上采用多反应监测正离子模式测定,外标法定量检测。结果蘑菇样本中检测出α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽和羧基二羟鬼笔毒肽4种蘑菇毒素,浓度分别为164、198、33、2208 mg/kg。结论本方法快速简便、准确,可用于因蘑菇毒素引起的食物中毒应急检测。

Objective To establish a method for rapid determination of 5 highly toxic mushroom toxins including α-amanitin, β-amanitin, γ-amanitin, phallacidin, phalloidin in poisonous mushrooms by ultra performance liquid chromatography-tandem mass spectrometry. Methods Ultrasonic extraction of methanol/water(3:7, V:V) mixture was performed. After centrifugation, the supernatant was separated by 0.22 μm microporous filtration membrane, and separated by C18 chromatographic column. It was determined by multi-reaction monitoring positive ion mode using ultra performance liquid chromatography-tandem mass spectrometer, and external standard method for quantitative detection. Results Four kinds of mushroom toxins were detected in the mushroom sample, namely, α-amanitin, β-amanitin, γ-amanitin, and phallacidin, with concentrations of 164, 198, 33, and 2208 mg/kg, respectively. Conclusion This method is rapid, simple and accurate, and is suitable for emergency detection of food poisoning caused by mushroom toxin.