磁性固相萃取净化-超高效液相色谱-串联质谱同时测定尿液中6种鹅膏肽类毒素  

Simultaneous determination of six kinds of amanita peptide toxins in urine by ultra performance liquid chromatography-tandem mass spectrometry with magnetic solid-phase extraction

作　　者：崔勇[1] 张冠英[1] 刘智[2] CUI Yong;ZHANG Guan-ying;LIU Zhi(Physical and Chemical Laboratory,Jilin Provincial Center for Sanitation Inspection and Test,Changchun,Jilin 130062,China)

机构地区：[1]吉林省卫生监测检验中心理化检验所,吉林长春130062 [2]长春中医药大学

出　　处：《中国卫生工程学》2024年第5期593-597,共5页Chinese Journal of Public Health Engineering

基　　金：吉林省卫生与健康技术创新项目(2020J097)。

摘　　要：目的建立磁性纳米材料萃取净化结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定尿液中α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、羧基二羟鬼笔毒肽、二羟鬼笔毒肽和羧基三羟鬼笔毒肽的检测方法。方法尿液样本经C18功能化磁性纳米颗粒(Fe3O_(4)@SiO_(2)@C18)的萃取净化,采用超高效液相色谱-串联质谱电喷雾电离(ESI),多反应监测(MRM)模式测定6种鹅膏肽类毒素。结果6种鹅膏肽类毒素的线性范围为0.50~50.00 ng/ml,均呈良好的线性关系;检出限为0.05~0.15μg/kg,定量限为0.15~0.50μg/kg,平均加标回收率为83.5%~102.3%之间,相对标准偏差(RSD)为2.55%~5.67%。结论该方法简便快速,结果准确可靠,适用于尿液中6种鹅膏肽类毒素检测。Objective To establish a method for the simultaneous determination ofα-amanitin,β-amanitin,γ-amanitin,phallacidin,phalloidin and phallisacin in urine by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with magnetic solid-phase extraction.Methods Urine samples were extracted and purified by C_(18)functionalized magnetic nanoparticles(Fe_3O_4@SiO_2@C_(18)).Six amanita peptide toxins were determined by a mass spectrometer coupled with electrospray ionization(ESI)and multiple reaction monitoring(MRM)mode.Results The linear range of six amanita peptide toxins was 0.50-50.00 ng/ml,and all showed good linear relationship.The limits of detection were 0.05-0.15μg/kg and the limits of quantification were 0.15-0.50μg/kg.The average recoveries of the method ranged from 83.5%to 102.3%,and the relative standard deviation(RSD)ranged from 2.55%to 5.67%.Conclusion The method is rapid,simple and accurate for the determination of six kinds of amanita peptide toxins in urine.

关 键 词：鹅膏肽类毒素 磁性固相萃取 尿液 超高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]