UPLC-MS/MS分析全血与尿液中氯胺酮、氟胺酮、溴胺酮残留

Determination of Ketamine,F-Ketamine and Br-Ketamine in whole blood and urine samples by UPLC-MS/MS

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.