基于超高效液相色谱-四极杆/静电场轨道离子阱高分辨质谱法的血液中30种芬太尼类物质检测方法的建立与验证  

Establishment and validation of ultra-performance liquid chromatography quadrupole electrostatic field orbitrap high-resolution mass spectrometry for the detection of 30 fentanyl-kind compounds in blood

作　　者：郭杰[1] 吕惊晗 张广华[2] 宋丽娟[2] 石辉丽 毕文姬 GUO Jie;LV Jinghan;ZHANG Guanghua;SONG Lijuan;SHI Huili;BI Wenji(Criminal Investigation Brigade,Qingdao Public Security Bureau,Qingdao 266034,China;Institute of Forensic Science,Ministry of Shandong Public Security,Jinan 250031,China;Criminal Investigation Brigade,Zibo Public Security Bureau,Zibo 255000,China)

机构地区：[1]青岛市公安局刑侦支队,青岛266034 [2]山东省公安厅物证检验鉴定中心,济南250031 [3]淄博市公安局刑侦支队,淄博255000

出　　处：《济宁医学院学报》2025年第1期1-7,共7页Journal of Jining Medical University

基　　金：山东省重点研发计划(重大科技创新工程)项目(2021CXGC011305)。

摘　　要：目的 建立超高效液相色谱-四极杆/静电场轨道离子阱高分辨质谱同时检测血液中30种芬太尼类物质的分析方法。方法 血液样品经甲醇-乙腈溶液提取过膜后,用高分辨率和高灵敏度的超高效液相色谱-四极杆/静电场轨道离子阱高分辨质谱进行检测分析。结果 30种芬太尼类物质在一定浓度范围内线性关系良好,相关系数(R^(2))均大于0.9970,检出限(LOD)和定量限(LOQ)分别在0.02~0.2ng/mL、0.1~0.5ng/mL;在0.5、2.0、10.0ng/mL 3个添加水平下,30种芬太尼类物质的回收率为80%~120%,基质效应80%~115%,日内和日间精密度1.6%~9.9%,准确度90%~110%。结论 通过实际样品检测验证,该方法在实际案件处理中的高效性和可靠性在公安机关办案及临床医学滥用药物研究方面具有很高的实用价值。Objective To establish a method for simultaneous determination of 30 fentanyl-related compounds in blood by ultra-performance liquid chromatography quadrupole electrostatic field orbital high resolution mass spectrometry(UPLC-Q Exactive Orbitrap HRMS).Methods Blood samples were extracted with methanol acetonitrile and detected by high-resolution and high-sensitivity UPLC-Q Exactive Orbitrap HRMS.Results There was a good linear relationship between the metabolites of 30 fentanyl-related substances in a certain concentration range,and the correlation coefficients(R2)were greater than 0.9970.The limits of detection(LOD)and limits of quantitation(LOQ)were 0.02~0.2ng/mL and 0.1~0.5ng/mL respectively.The recoveries of 30 fentanyl-related substances were 80%~120%,the matrix effect was 80%~115%,and the RSD%of intra-day and inter-day precision were 1.6%and 9.9%.At three different levels of 0.5,2.0 and 10.0ng/mL,the accuracy was between 90%and 110%.Conclusion The method was validated through sample detection and demonstrated high efficiency and raliability in practical case handling.It has significant practical value for case investigation by public security organs and research on drug abuse in clinical medicine.

关 键 词：超高效液相色谱四极杆/静电场轨道离子阱高分辨质谱 血液 芬太尼类物质 

分 类 号：R895[医药卫生—法医学]