UPLC-Q/Exactive MS快速筛查人体血液中21种生物碱  

Rapid screening of 21 alkaloids in blood by UPLC-Q/Exactive MS

作　　者：罗敬锋[1] 王力春[1] 石银涛[1] 李恒[1] 先有其 郑经[1] 王俊伟[1] Luo jingfeng;Wang Lichun;ShiYintao;Li Heng;Xian youqi;Zheng Jing;Wang Junwei(Institute of Forensic Science,Chongqing Public Security Bureau,Chongqing 400707,China;Thermo Flsher Scientific(China),Shanghai 201203,China)

机构地区：[1]重庆市公安局物证鉴定中心,重庆400707 [2]赛默飞世尔科技(中国)有限公司,上海201203

出　　处：《中国法医学杂志》2021年第4期423-425,429,共4页Chinese Journal of Forensic Medicine

基　　金：2018年度公共安全行业标准制修订计划(201870136)。

摘　　要：目的建立了超高效液相色谱-四级杆/静电场轨道阱高分辨质谱(UPLC-Q/Exactive MS)快速筛查血液中21种生物碱的方法。方法样品经乙腈蛋白沉淀法进行前处理。目标物经ACQUITY UPLC@BEHC18分离,以乙腈及5mmol/L甲酸铵(含0.1%甲酸)水溶液进行梯度洗脱,在电喷雾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,根据21种生物碱的高分辨分子离子峰、同位素分布、特征子离子信息建立数据库,采用Trace Finder 4.1软件实现定性检索。结果人体血液中21种生物碱的检出限(LOD)在1.0-20.0ng/m L之间,用Trace Finder软件对血液样品中添加的21中生物碱进行快速筛查,通过数据库比对,目标化合物均被检出。结论方法操作简便,准确性好,灵敏度高,适用于血液中生物碱的快速筛查。Objective An analytical method was developed to determine 21 alkaloids in blood by ultra performance liquid chromatography quadrupole/orbitrap high resolution mass spectrometry(UPLC-Q/Exactive MS) in blood. Mthods The spiked samples were pretreated by protein precipitation with acetonitrile, thereby having the target compound separated from ACQUITY UPLC@BEHC18 column that was flowed through gradient elution of acetonitrile, and 5 mmol/L ammonium aormate solution containing 0.1%(v/v) formic acid as mobile phase’s elution with a flow rate of 0.3 mL/min. The alkaloids were analyzed by full MS scan/data dependent MS2(Full MS/dd-MS2) mode by electrospray ionsource. According to some parameters of molecular ion, isotopic ion ratios, characteristic product ion, the searched database was built with the Trace Finder 4.1 software and then used for the analysis of spiked samples. Results The limit of detection(LOD) for 21 alkaloids in human blood was in the range of 1.0-20.0 ng/mL. The spiked compounds were all detected by the established database fromTrace Finder software. Conclusions The results indicated that this method is simple, reliable and sensitive and suitable for the screening of alkaloids in blood.

关 键 词：超高效液相色谱/静电场轨道阱高分辨质谱 血液 生物碱 快速筛查 

分 类 号：TJ012.4[兵器科学与技术—兵器发射理论与技术]