法医学杂志

法医学杂志 ›› 2024, Vol. 40 ›› Issue (6): 564-568.DOI: 10.12116/j.issn.1004-5619.2024.340202

所属专题： 高分辨质谱技术专题

• 高分辨质谱技术专题 • 上一篇    下一篇

UPLC-Q/Orbitrap HRMS对全血中60种天然毒素的快速筛查

郭铸涛1,2(), 邓乾亚1, 何思阳1, 郑水庆1,3, 汪蓉1, 孙文娟1, 梁晨1,3(), 倪春芳1,3()   

  1. 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
  • 收稿日期:2024-02-05 发布日期:2025-03-10 出版日期:2024-12-25
  • 通讯作者: 梁晨,倪春芳
  • 作者简介:郭铸涛（1998—），男，硕士研究生，主要从事药物分析研究；E-mail：21211030072@m.fudan.edu.cn
  • 基金资助:
    上海市“科技创新行动计划”社会发展科技攻关定向项目(21dz1200301)

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

Zhu-tao GUO1,2(), Qian-ya DENG1, Si-yang HE1, Shui-qing ZHENG1,3, Rong WANG1, Wen-juan SUN1, Chen LIANG1,3(), Chun-fang NI1,3()   

  1. 1.Shanghai Key Laboratory of Crime Scene Evidence, Institute of Forensic Science, Shanghai Public Security Bureau, Shanghai 200083, China
    2.School of Pharmacy, Fudan University, Shanghai 201203, China
    3.Shanghai Police College, Shanghai 200137, China
  • Received:2024-02-05 Online:2025-03-10 Published:2024-12-25
  • Contact: Chen LIANG, Chun-fang NI

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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 GOLDTM C18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-MS2）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20 ng/mL）和毒毛旋花子苷元（LOD为40 ng/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。

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

Abstract:

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 ultrasonic-assisted dispersion, and then a Hypersil GOLDTM C18 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-MS2） 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.

Key words: forensic medicine, toxicological analysis, ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry （UPLC-Q/Orbitrap HRMS）, natural toxin, whole blood, rapid screening

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