UPLC-Q/Orbitrap HRMS对全血中60种天然毒素的快速筛查  

Rapid Screening of 60 Types of Natural Toxins in Whole Blood by UPLC-Q/Orbitrap HRMS

作　　者：郭铸涛 邓乾亚 何思阳[1] 郑水庆[1,3] 汪蓉 孙文娟[1] 梁晨 倪春芳[1,3] GUO Zhu-tao;DENG Qian-ya;HE Si-yang;ZHENG Shui-qing;WANG Rong;SUN Wen-juan;LIANG Chen;NI Chun-fang(Shanghai Key Laboratory of Crime Scene Evidence,Institute of Forensic Science,Shanghai Public Secu-rity Bureau,Shanghai 200083,China;School of Pharmacy,Fudan University,Shanghai 201203,China;Shanghai Police College,Shanghai 200137,China)

机构地区：[1]上海市公安局物证鉴定中心、上海市现场物证重点实验室,上海200083 [2]复旦大学药学院,上海201203 [3]上海公安学院,上海200137

出　　处：《法医学杂志》2024年第6期564-568,共5页Journal of Forensic Medicine

基　　金：上海市“科技创新行动计划”社会发展科技攻关定向项目(21dz1200301)。

摘　　要：目的采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry,UPLC-Q/Orbitrap HRMS)技术建立全血中60种天然毒素的快速筛查方法。方法分析并记录60种天然毒素标准品的色谱和质谱信息,构建筛查数据库。全血用蛋白沉淀法配合超声辅助分散进行前处理,使用Hypersil GOLD^(TM)C_(18)色谱柱,以5 mmol/L甲酸铵水溶液(含0.1%甲酸)和乙腈为流动相进行梯度洗脱,在电喷雾电离正离子模式和全扫描/数据依赖二级扫描(Full MS/dd-MS^(2))模式下检测。基于构建的筛查数据库,采用TraceFinder软件实现全血中60种天然毒素的快速筛查。结果建立的全血中60种天然毒素的UPLC-Q/Orbitrap HRMS筛查方法,除氧化苦参碱(LOD为20ng/mL)和毒毛旋花子苷元(LOD为40ng/mL)外,其余58种天然毒素的LOD范围为0.05~5 ng/mL。结论该方法前处理简单、高效,可以实现对全血中60种天然毒素的快速筛查。Objective To establish a rapid screening method for 60 types of natural toxins in whole blood by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q/Orbitrap HRMS).Methods The chromatographic and mass spectrometric information of 60 standard samples of natural toxins were analyzed and recorded,and a screening database was built.Whole blood was pretreated by protein precipitation method combined with ultrasonicassisted dispersion,and then a Hypersil GOLD^(TM)C_(18)column was used with 5 mmol/L ammonium formate aqueous solution(containing 0.1%formic acid)and acetonitrile as mobile phase for gradient elution.In the positive ion mode,the data were collected in full scan/data-dependent secondary scan(Full MS/dd-MS^(2))mode.Based on the established screening library,the rapid screening of 60 types of natural toxins in whole blood was realized by TraceFinder software.Results A UPLC-Q/Orbitrap HRMS method was developed for the screening of 60 types of natural toxins in whole blood.Except for the limit of detection(LOD)of oxymatrine(20 ng/mL)and strophanthidin(40 ng/mL),the LOD for the other 58 natural toxins was in the range of 0.05-5 ng/mL.Conclusion This method has a simple and efficient pretreatment process and can achieve rapid screening of 60 types of natural toxins in whole blood.

关 键 词：法医学 毒物分析 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UPLC-Q/Qrbitrap HRMS) 天然毒素 全血 快速筛查 

分 类 号：R89[医药卫生—法医学] DF795.1[医药卫生—临床医学] D919.1[政治法律—诉讼法学]