Hebei Key Laboratory of Forensic Medicine, Collaborative Innovation Center of Forensic Medical Molecular Identification, Forensic Identification Center of Hebei Medical University, College of Forensic Medicine, Hebei Medical University, Shijiazhuang 050017, China.
College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China.
Fa Yi Xue Za Zhi. 2021 Oct 25;37(5):646-652. doi: 10.12116/j.issn.1004-5619.2020.301001.
To develop a method for the simultaneous and rapid detection of five mushroom toxins (α-amanitin, phallacidin, muscimol, muscarine and psilocin) in blood by ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS).
The blood samples were precipitated with acetonitrile-water solution(∶=3∶1) and PAX powder, then separated on ACQUITY Premier C column, eluted gradient. Five kinds of mushroom toxins were monitored by FullMS-ddMS/positive ion scanning mode, and qualitative and quantitative analysis was conducted according to the accurate mass numbers of primary and secondary fragment ions.
All the five mushroom toxins had good linearity in their linear range, with a determination coefficient ()≥0.99. The detection limit was 0.2-20 ng/mL. The ration limit was 0.5-50 ng/mL. The recoveries of low, medium and high additive levels were 89.6%-101.4%, the relative standard deviation was 1.7%-6.7%, the accuracy was 90.4%-101.3%, the intra-day precision was 0.6%-9.0%, the daytime precision was 1.7%-6.3%, and the matrix effect was 42.2%-129.8%.
The method is simple, rapid, high recovery rate, and could be used for rapid and accurate qualitative screening and quantitative analysis of various mushroom toxins in biological samples at the same time, so as to provide basis for the identification of mushroom poisoning events.
建立一种超高效液相色谱-高分辨质谱法（UPLC-HRMS）同时快速检测血液中 5 种蘑菇毒素（α-鹅膏蕈碱、鹅膏蕈氨酸、蝇蕈醇、毒蕈碱和裸盖菇素）的方法。
用乙腈-水（∶=3∶1）和 PAX 粉末沉淀血液样品，然后在 ACQUITY Premier C 柱上进行分离，采用梯度洗脱。采用全扫描-数据依赖子离子扫描模式（FullMS-ddMS/positive ion scanning mode）监测 5 种蘑菇毒素，根据一级和二级碎片离子的精确质量数进行定性和定量分析。
5 种蘑菇毒素在其线性范围内均具有良好的线性关系，决定系数（）≥0.99。检测限为 0.2-20 ng/mL，定量限为 0.5-50 ng/mL。低、中、高添加水平的回收率为 89.6%-101.4%，相对标准偏差为 1.7%-6.7%，准确度为 90.4%-101.3%，日内精密度为 0.6%-9.0%，日间精密度为 1.7%-6.3%，基质效应为 42.2%-129.8%。
该方法简单、快速、回收率高，可用于同时快速准确地定性筛选和定量分析生物样品中的各种蘑菇毒素，为蘑菇中毒事件的鉴定提供依据。
