在线液相色谱-二极管阵列检测器-串联质谱法检测野生菌中鹅膏毒肽和鬼笔毒肽

引用本文: 徐小民, 张京顺, 蔡增轩, 张晶, 黄百芬, 许娇娇, 陈苘. 在线液相色谱-二极管阵列检测器-串联质谱法检测野生菌中鹅膏毒肽和鬼笔毒肽[J]. 色谱, 2017, 35(6): 613-619. doi: 10.3724/SP.J.1123.2017.02008 shu

Citation: XU Xiaomin, ZHANG Jingshun, CAI Zengxuan, ZHANG Jing, HUANG Baifen, XU Jiaojiao, CHEN Qing. Determination of amanitins and phallotoxins in wild mushrooms by online liquid chromatography-diode array detector-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(6): 613-619. doi: 10.3724/SP.J.1123.2017.02008 shu

在线液相色谱-二极管阵列检测器-串联质谱法检测野生菌中鹅膏毒肽和鬼笔毒肽

浙江省疾病预防控制中心, 浙江杭州 310051
基金项目:
浙江省医药卫生科技计划项目（2015DTA006）.

摘要: 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XBridge^TM 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。

关键词:

English

Determination of amanitins and phallotoxins in wild mushrooms by online liquid chromatography-diode array detector-tandem mass spectrometry

Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China
Received Date: 09 February 2017
Fund Project:
Science Research Foundation Program of Zhejiang Provincial Medicine and Health (No. 2015DTA006).

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 XBridge^TM 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.

Key words:

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

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在线液相色谱-二极管阵列检测器-串联质谱法检测野生菌中鹅膏毒肽和鬼笔毒肽

English

Determination of amanitins and phallotoxins in wild mushrooms by online liquid chromatography-diode array detector-tandem mass spectrometry

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在线液相色谱-二极管阵列检测器-串联质谱法检测野生菌中鹅膏毒肽和鬼笔毒肽

English

Determination of amanitins and phallotoxins in wild mushrooms by online liquid chromatography-diode array detector-tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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