Tomková Jana, Ondra Peter, Válka Ivo
Department of Forensic Medicine and Medical Law, University Hospital Olomouc, Hněvotínská 3, 775 09 Olomouc, Czech Republic.
Department of Forensic Medicine and Medical Law, University Hospital Olomouc, Hněvotínská 3, 775 09 Olomouc, Czech Republic.
Forensic Sci Int. 2015 Jun;251:209-13. doi: 10.1016/j.forsciint.2015.04.007. Epub 2015 Apr 14.
This paper presents a method for the simultaneous determination of α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction (SPE) and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. The method can be used for a diagnostics of mushroom poisonings. Different SPE cartridges were tested for sample preparation, namely hydrophilic modified reversed-phase (Oasis HLB) and polymeric weak cation phase (Strata X-CW). The latter gave better results and therefore it was chosen for the subsequent method optimization and partial validation. In the course of validation, limits of detection, linearity, intraday and interday precisions and recoveries were evaluated. The obtained LOD values of α-amanitin and β-amanitin were 1ng/mL and of muscarine 0.09ng/mL. The intraday and interday precisions of human urine spiked with α-amanitin (10ng/mL), β-amanitin (10ng/mL) and muscarine (1ng/mL) ranged from 6% to 10% and from 7% to 13%, respectively. The developed method was proved to be a relevant tool for the simultaneous determination of the studied mushroom toxins in human urine after mushroom poisoning.
本文介绍了一种通过固相萃取（SPE）和超高效液相色谱联用超高分辩率飞行时间质谱同时测定人尿液中α-鹅膏毒肽、β-鹅膏毒肽和毒蕈碱的方法。该方法可用于蘑菇中毒的诊断。对不同的SPE柱进行了样品制备测试，即亲水改性反相柱（Oasis HLB）和聚合物弱阳离子柱（Strata X-CW）。后者效果更好，因此被选用于后续方法优化和部分验证。在验证过程中，评估了检测限、线性、日内和日间精密度以及回收率。所获得的α-鹅膏毒肽和β-鹅膏毒肽的检测限为1ng/mL，毒蕈碱的检测限为0.09ng/mL。添加了α-鹅膏毒肽（10ng/mL）、β-鹅膏毒肽（10ng/mL）和毒蕈碱（1ng/mL）的人尿液的日内和日间精密度分别为6%至10%和7%至13%。已证明所开发的方法是一种用于在蘑菇中毒后人尿液中同时测定所研究蘑菇毒素的相关工具。
