Abstract:Objective To develop an analytical method of ibotenic acid (IBA) and muscimol (MUS) in wild mushroom by dansyl chloride (DNSCl) derivatization-liquid chromatography-tandem mass spectrometry (LC-MS/MS), and to provide technical support for etiological identification of mushroom poisoning events. Methods The sample was extracted with hydrochloric acid solution, derived by bimolecular DNSCl, diluted and inorganic salts precipitated with acetonitrile. The extract was separated by a waters XBridgeTM BEH C18 column and measured by LC-MS/MS. Results The limits of detection for IBA and MUS in wild mushroom were 0.15 mg/kg and 0.1 mg/kg, respectively. Good linear relationship was obtained for IBA and MUS at the range of 0.5-250 mg/kg with the correlation coefficient of 0.997 and 0.999, respectively. The average recoveries at three spiking levels were 84.5%-102.0% with relative standard deviations (RSDs, n=6) of 4.7%-8.6% for IBA. The average recoveries were 88.6%-95.4% with RSDs (n=6) of 4.9%-7.5% for MUS. Conclusion The optimized sample extraction and bimolecular DNSCl derivatization conditions can achieve rapid and accurate analysis of IBA and MUS in wild mushroom poisoning sample.
[1] GOVORUSHKO S,REZAEE R,DUMANOV J,et al.Poisoning associated with the use of mushrooms:a review of the global pattern and main characteristics[J].Food Chem Toxicol,2019,128:267-279. [2] LI H,ZHANG H,ZHANG Y,et al.Mushroom poisoning outbreaks-China,2019[J].China CDC Weekly,2020,2(2):19-24. [3] MOSS M J,HENDRICKSON R G.Toxicity of muscimol and ibotenic acid containing mushrooms reported to a regional poison control center from 2002-2016[J].Clin Toxicol(Phila),2019,57:99-103. [4] 章轶哲,孙承业,李海蛟,等.一起蘑菇致急性中毒事件的现场调查与鉴定[J].中华急诊医学杂志,2016,25(8):1012-1015. [5] LUMPERT M,KREFT S.Catching flies with Amanita muscaria:traditional recipes from Slovenia and their efficacy in the extraction of ibotenic acid[J].J Ethnopharmacol,2016,187:1-8. [6] XU X M,CAI Z X,ZHANG J S,et al.Analysis of monofluoroacetic acid in urine by liquid chromatography-triple quadrupole mass spectrometry and preparation of the positive sample by the bioconversion from monofluoroacetamide to monofluoroacetic acid in vitro[J].J Chromatogr B,2016,1027:131-138. [7] GINTEROVA P,SOKOLOVA B,ONDRA P,et al.Determination of mushroom toxins ibotenic acid,muscimol and muscarine by capillary electrophoresis coupled with electrospray tandem mass spectrometry[J].Talanta,2014,125:242-247. [8] GONMORI K,HASEGAWA K,FUJITA H,et al.Analysis of ibotenic acid and muscimol in Amanita mushrooms by hydrophilic interaction liquid chromatography-tandem mass spectrometry[J].Forensic Toxicol,2012,30:168-172. [9] HASEGAWA K,GONMORI K,FUJITA H,et al.Determination of ibotenic acid and muscimol,the Amanita mushroom toxins,in human serum by liquid chromatography-tandem mass spectrometry[J].Forensic Toxicol,2013,31:322-327. [10] TSUJIKAWA K,KUWAYAMA K,MIYAGUCHI H,et al.Determination of muscimol and ibotenic acid in Amanita mushrooms by high-performance liquid chromatography and liquid chromatography-tandem mass spectrometry[J].J Chromatogr B,2007,852:430-435. [11] 伍福仙,张志清,王瑾,等.超高效液相色谱串联四级杆飞行时间质谱法检测毒蘑菇中4种常见毒素含量[J].食品安全质量检测学报,2019,10(22):7656-7664. [12] MARTINS R S,ANTUNES N J,COMERLATTI G,et al.Quantification of estradiol cypionate in plasma by liquid chromatography coupled with tandem mass spectrometry:application in a pharmacokinetic study in healthy female volunteers[J].J Pharm Biomed Anal,2019,170:273-278. [13] WANG Z,YU J,YAO J,et al.Simultaneous identification and quantification of bisphenol A and 12 bisphenol analogues in environmental samples using precolumn derivatization and ultra high performance liquid chromatography with tandem mass spectrometry[J].J Sep Sci,2018,41:2269-2278. [14] 赵昂,张航,姚迪,等.超快速液相色谱-串联质谱法检测人血清中雌酮、雌二醇及雌三醇的方法学研究[J].中国科技论文,2016,11(18):2062-2068. [15] GUO K,LI L.Differential 12C-/13C-isotope dansylation labeling and fast liquid chromatography/mass spectrometry for absolute and relative quantification of the metabolome[J].Anal Chem,2009,81:3919-3932.