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作 者:方雅莉 马骥 张磊 Fang Yali;Ma Ji;Zhang Lei(Scientific Research Platform Service Management Center,Guangdong Medical University Guang Dong Dong Guan 523000;Forensic Science Center of DongGuan Public Security Department,Guang Dong Dong Guan 523000)
机构地区:[1]广东医科大学科研平台服务管理中心,广东东莞523000 [2]东莞市公安局物证鉴定中心,广东东莞523000
出 处:《中国法医学杂志》2023年第1期53-56,62,共5页Chinese Journal of Forensic Medicine
基 金:广东医科大学青年培育基金自然科学类面上项目(GDMUQ2021050);广东省公安厅科技攻关项目(2022GDSSGG15,2022GDSSGG16)。
摘 要:目的建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定人的血液、尿液样品中氯胺酮、氟胺酮、溴胺酮残留的方法。方法空白血、空白尿样品中加入氯胺酮、氟胺酮和溴胺酮标准溶液,使用乙腈沉淀蛋白法作为前处理方式,采用UPLC-MS/MS检测。质谱检测采用正离子扫描,多反应离子监测模式(MRM)。定性定量均以氯胺酮、氟胺酮、溴胺酮母离子和子离子进行分析。结果在0.001、0.050、0.500 mg/L三个添加水平下,氯胺酮、氟胺酮、溴胺酮在空白血、空白尿液样品中的回收率在71.02%~133.68%之间,相对标准偏差在0.28%~13.19%之间,定量限均为0.001 mg/L,检出限均为0.0005 mg/L。结论该方法灵敏度高、分析速度快、操作简便。Objective A method was developed for the qualitative and quantitative analysis of Ketamine,F-Ketamine and Br-Ketamine by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Blank whole blood and blank urine were spiked with Ketamine,F-Ketamine and Br-Ketamine standards and precipitated protein by vortex and centrifugation.Extracts was analyzed by UPLC-MS/MS in positive ionization and multiple reaction monitoring(MRM)mode.The parent ion and two daughter ions of Ketamine,F-Ketamine and Br-Ketamine were used for qualification and quantification.Results The recoveries of Ketamine,F-Ketamine and Br-Ketamine ranged from 71.02%to 133.68%with the spiked levels of 0.001,0.050 and 0.500 mg/L,respectively.The relative standard deviation(RSD)ranged from 0.28%to 13.19%,the limits of quantification(LOQs)were 0.001 mg/L,and the limits of detection(LODs)were 0.0005 mg/L.Conclusion This method was proved to be sensitive,effective and simple.
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