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[在线液相色谱-二极管阵列检测器-串联质谱法测定野生蘑菇中的鹅膏毒素和鬼笔毒素]

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

作者信息

Xu Xiaomin, Zhang Jingshun, Cai Zengxuan, Zhang Jing, Huang Baifen, Xu Jiaojiao, Chen Qing

机构信息

Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China.

出版信息

Se Pu. 2017 Jun 8;35(6):613-619. doi: 10.3724/SP.J.1123.2017.02008.

Abstract

A fast and wide linear range method was established for the determination of mushroom toxins amanitins (-amanitin,-amanitin and -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 BEH C 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 and white .

摘要

建立了一种快速且线性范围宽的方法,用于通过在线液相色谱 - 二极管阵列检测器 - 串联质谱法(LC - DAD - MS/MS)测定野生蘑菇中的蘑菇毒素鹅膏菌素(α-鹅膏菌素、β-鹅膏菌素和γ-鹅膏菌素)和鬼笔毒素(鬼笔环肽和鬼笔毒环肽)。蘑菇毒素用甲醇提取,然后用水稀释。提取物在XBridge BEH C18柱(150 mm×3.0 mm,2.5 μm)上于pH 10.7条件下分离,通过DAD测定,然后用MS/MS分析。采用碱性流动相条件以提高氢离子加合物的电离效率。在15分钟内实现了分析物的基线分离。样品基质的检测限(LOD)为0.005 - 0.02 mg/kg。当毒素含量小于2 mg/kg时,通过MS/MS测定结果对毒素进行定量;当含量大于2 mg/kg时,通过DAD获得的结果进行定量。该方法一次进样的线性范围为0.05 - 500 mg/kg。该方法成功应用于[具体蘑菇种类1]和白[具体蘑菇种类2]中鹅膏菌素和鬼笔毒素的分析。

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