Analysis of Five Mushroom Toxins in Blood by UPLC-HRMS / 法医学杂志

OBJECTIVES@#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).@*METHODS@#The blood samples were precipitated with acetonitrile-water solution(Vacetonitril∶Vwater=3∶1) and PAX powder, then separated on ACQUITY Premier C18 column, eluted gradient. Five kinds of mushroom toxins were monitored by FullMS-ddMS2/positive ion scanning mode, and qualitative and quantitative analysis was conducted according to the accurate mass numbers of primary and secondary fragment ions.@*RESULTS@#All the five mushroom toxins had good linearity in their linear range, with a determination coefficient (R2)≥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%.@*CONCLUSIONS@#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.

Analysis of Common Herbicides in Blood by UPLC-HRMS / 法医学杂志

Objective To develop a method to screen and quantify 10 common herbicides (paraquat, diquat, glyphosate, glufosinate, cyanazine, atrazine, metazachlor, acetochlor, chlorsulfuron, and metsulfuron) in blood.Methods With acetonitrile-water solution[V (acetonitrile) ∶V (water) =3∶1]as protein precipitant, 10 common herbicides in blood were detected using ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS).Results All the 10 herbicides had good linearity in their linear range (coefficient of determination R2≥0.993), with the recovery rates 67.4％-111.9％, the relative standard deviations 1.5％-10.8％, the accuracies 85.1％-106.1％, intra-day precisions 2.7％-13.5％, and inter-day precisions 3.3％-13.3％.Conclusion This method is easy to operate with high recovery rates.It enables rapid and accurate qualitative screening and quantitative analysis of various herbicides in blood simultaneously.