超高效液相色谱三重四极杆质谱联用法快速检测尿液和血浆中鹅膏毒肽和鬼笔毒肽  

Rapid Simultaneous Determination of Five Amatoxins and Phallotoxins in Human Urine and Plasma by Ultra Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry

作　　者：张秀尧[1] 蔡欣欣[1] 

机构地区：[1]温州市疾病预防控制中心,温州325001

出　　处：《分析化学》2010年第1期39-44,共6页Chinese Journal of Analytical Chemistry

基　　金：温州市医学重点学科;温州市第三轮"311"工程建设项目基金(No.2008012)资助

摘　　要：建立了同时快速检测尿液和血浆中3种鹅膏毒肽和2种鬼笔毒肽的超高效液相色谱三重四极杆质谱联用分析方法。尿液样品直接进样,血浆样品经乙腈沉淀除蛋白后,在UPLCHSST3色谱柱上分离,正离子电喷雾多反应监测(MRM)模式检测,基体匹配标准外标法定量。尿液和血浆样品的线性范围分别为2～100和1～100μg/L;加标回收率分别在92.0%～108.0%和85.0%～100.0%的范围内;相对标准偏差为1.0%～22.0%和2.0%～22.0%(n=6);样品的检出限为0.2～1.0μg/L和0.1～0.5μg/L(S/N=3)。本方法灵敏,简单,快速,特异性强。Specific detection of amatoxins and phallotoxins in body fluids is necessary for an early diagnosis of an intoxication with mushrooms.In this study,a rapid method for the simultaneous determination of α-,βand γ-amanitin,phalloidin and phallacidin in human urine and plasma was first developed by ultra-performance liquid chromatography-tandem mass spectrometry.Urine sample was directly injected into the separation system and plasma sample was initially prepared by precipitation of proteins with 1% acetic acid in acetonitrile.The toxin was analyzed on an ACQUITY UPLC HSS T3 column using a gradient program with a cycle time of 9 min,and detected by positive electrospray ionization tandem mass spectrometry in the MRM mode,and quantified by matrix-match standard solution.The detection limits（S/N=3） of the toxins were within 0.2-1 μg/L and 0.1-0.5 μg/L for urine and plasma,respectively.The standard curves were linear in the range of 2-100 μg/L for urine and 1-100 μg/L for plasma.The average recoveries were 92.0%-108.0% and 85.0%-100.0% for the toxins spiked in urine and plasma,with RSDs of 1.0%-22.0% and 2.0% 22.0% （n=6）,respectively.The method was simple,selective and sensitive to detect the amatoxins and phallotoxins in urine and plasma for both clinical and forensic purposes.

关 键 词：超高效液相色谱三重四极杆质谱法 鹅膏毒肽 鬼笔毒肽 尿液 血浆 

分 类 号：R114[医药卫生—卫生毒理学]