超高效液相色谱-串联质谱法快速测定蘑菇中5种鹅膏肽类毒素

Rapid determination of 5 kinds of amanita peptide toxins in mushrooms by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱串联质谱  鹅膏肽类毒素  蘑菇

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  amanita peptide toxins  mushrooms

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速测定鲜蘑菇中α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、二羟鬼笔毒肽和羧基二羟鬼笔毒肽5种强毒性鹅膏肽类毒素的检测方法。方法 样品经充分粉碎后, 加入10%甲醇超声提取后, 离心上清液过0.22 μm微孔滤膜, 用Waters Xselect CSH C18 (2.1 mm×100 mm, 1.7 μm)色谱柱分离, 外标法定量。结果 在优化条件下, 该方法中5种强毒性鹅膏肽类毒素的最低检出限均为0.02 mg/kg, 定量限为0.06 mg/kg, 平均回收率为78.2%~103.5%, 相对标准偏差为3.1%~7.6%。结论 本方法简便、快速、准确, 回收率好, 适用于因鹅膏肽类毒素引起的食物中毒快速应急检测。

英文摘要:

      Objective To establish a method for the rapid determination of 5 kinds of highly toxic amanita peptide toxins including α-amanitin, β-amanitin, γ-amanitin, phalloidin and phallacidinin in mushrooms by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After thorough crushing of the sample, 10% methanol was added for ultrasonic extraction. The supernatant was centrifuged and passed through a 0.22 μm microporous membrane using Waters Xselect CSH C18 (2.1 mm×100 mm, 1.7 μm) chromatographic column separation, quantitative analysis using external standard method. Results Under optimized conditions, the lowest limits of detection and limits of quantification of 5 kinds of highly toxic peptide toxins in this method were 0.02 mg/kg and 0.06 mg/kg, respectively. The average recovery rates were 78.2%–103.5%, and the relative standard deviations were 3.1%–7.6%. Conclusion This method is simple, fast, accurate, with good recovery rate, and is suitable for rapid emergency detection of food poisoning caused by amanita peptide toxins.