Yifu Jiang,Le Lang,Jingwen Zhang,Yining Ji,Chenglong Zhang,Ruiqin Yang,Xuwen Li
This study combined the structural characteristics of amanita peptide toxins to prepare a Fe 3 O 4 /P4VPBA/PPy/GO composite material as a magnetic solid-phase extraction adsorbent. The experimental results indicated that this adsorbent showed excellent selectivity for the extraction of amatoxins and phallotoxins from mushroom samples. Compared with traditional dispersive solid-phase extraction, this adsorbent enables rapid separation in the enrichment and elution recovery stages through the application of a magnetic field . Simultaneously, the study optimized the conditions for ultraperformance liquid chromatography–mass spectrometry (UPLC–MS/MS), ensuring both separation efficiency and accuracy while reducing the analysis time. The researchers established the MSPE–UPLC–MS/MS method for the determination of amanita peptide toxins in wild mushrooms. This method not only simplified and expedited the sample pretreatment process but also achieved qualitative and quantitative analyses in a short period, thus demonstrating high detection sensitivity and outstanding recovery rates. Furthermore, the developed method was successfully applied to analyze toxic mushrooms discovered in Nanjing, China. The potential for extensive utilization of this method is highlighted in the field of food analysis and detection.
Mushroom poisoning is becoming a serious food safety and public health issue due to its high morbidity and mortality in some parts of the world. Identifying mushroom toxins at an early stage of suspected intoxication is crucial for therapeutic decision making. Ibotenic acid, muscimol, 2-amino-4,5-hexadienoic acid and 2-amino-4-pentynoic acid are a group of amino group-containing mushroom toxins that can lead to hallucination and neurotoxicity on humans. However, there is no method established for simultaneous detection of the four toxins. In this present study, a new derivatization method was developed for the determination of these toxins in mushroom and urine samples by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). After sample extraction the extract was directly derivatized by using 9-fluorenylmethyloxycarbonyl chloride and multiple factors affecting derivatization reaction were systematically optimized to enhance method sensitivity. Furthermore, liquid-liquid extraction with dichloromethane was employed for purification of the derivatized products. The method was fully validated for linearity, sensitivity, recovery and precision. Recoveries of four mushroom toxins were in the range of 85%–101% for urine and 82%–108% for mushroom. The limits of quantification were from 0.05 to 1 μg/L in urine and 1–20 μg/kg in mushroom. In addition, the developed method was successfully applied on mushroom samples treated by cooking and digesting with artificial gastric juice, demonstrating that vomitus as well as cooked mushroom and its soup can be used as the valuable materials for identifying mushroom poisoning caused by these four toxins.
Bo Zhang,Yang Liu,Shengnan Li,Ruonan Li,Yunhui Zhang,Hua Zhao
Wild mushroom poisoning is an emerging global food safety issue, especially in subtropical regions like southwestern China, where incidents are geographically clustered. Current detection methods are often time-consuming and overlook region-specific toxins. We developed a rapid, sensitive, and accurate method for the simultaneous detection of ten characteristic mushroom toxins prevalent in Guizhou, China. The method combines graphite multi-walled carbon nanotubes (G-MWCNTs) for sample preparation with Orbitrap high-resolution mass spectrometry (HRMS). Wild mushroom samples were extracted via ultrasonic-assisted methanol–water extraction, purified using G-MWCNTs, and separated on a Hypersil GOLD C18 column (100 mm × 2.1 mm, 1.9 μm). Gradient elution was performed with 0.1% formic acid + 0.01% ammonia and acetonitrile; quantification used the external standard method. The method achieved LODs of 0.005–0.2 mg/kg and LOQs of 0.015–0.6 mg/kg, with RSDs below 18.11% and excellent linearity (R2= 0.9936–0.9989). Among 45 wild mushroom samples, toxin levels ranged from 0.032 to 445.10 mg/kg, with a detection rate of 22.22%, suggesting notable poisoning risk. This method reduces pretreatment time while ensuring high analytical performance, offering a reliable tool for rapid toxin screening and supporting regional surveillance of wild mushroom poisoning.
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