HPLC-MS/MS法测定尿液中的氟胺酮及其代谢物
Determination of 2-fluoro-deschloroketamine and Its Metabolites in Urine by HPLC-MS/MS
马俊 1李冬梅 1夏梦婵 1陈军 2赵一哲 1万耔莘 1朱孔文 3赵霞 1郑珲2
作者信息
- 1. 国家毒品实验室北京分中心,北京 100164
- 2. 公安部禁毒情报技术中心,毒品监测管控与禁毒关键技术公安部重点实验室,北京 100193
- 3. 法庭毒物分析公安部重点实验室,北京 100192
- 折叠
摘要
本文确定了除去甲氟胺酮以外的两种氟胺酮一相代谢产物的具体结构,并建立了尿液中氟胺酮、去甲氟胺酮、顺式氟胺醇和反式氟胺醇的高效液相色谱-三重四极杆串联质谱(HPLC-QQQ MS/MS)检测方法.基于液相色谱串联高分辨质谱筛查,定向合成两种氟胺酮代谢物顺式氟胺醇和反式氟胺醇,并利用1H NMR、13C NMR和二维NOE谱图确定其结构;建立了尿液中氟胺酮、去甲氟胺酮、顺式氟胺醇和反式氟胺醇的HPLC-QQQ MS/MS检验方法,该方法对于氟胺酮及其三种主要代谢物在0.5～200 ng/mL浓度范围内线性关系良好,线性相关系数均大于0.996 3,方法回收率介于81.60％～119.33％之间;利用所建方法对吸毒人员尿液样本中的氟胺酮及其三种代谢物的含量进行了检测.本研究所开发的方法检出限低、回收率高和重现性好,可用于定性和定量氟胺酮的稳定代谢物.
Abstract
In this paper,the specific structures of two first-phase metabolites of 2-fluoro-deschloroketamine except nor-2-fluoro-deschloroketamine were determined,and a detection method of 2-fluoro-deschloroketamine,nor-2-fluoro-deschloroketamine,cis-Dihydro-2-fluoro-deschloroketamine and trans-Dihydro-2-fluoro-deschloroketamine in urine was estabished using HPLC-QQQ MS/MS.Through HPLC-HRMS screening,two metabolites of 2-fluoro-deschloroketamine,namely cis-Dihydro-2-fluoro-deschloroketamine and trans-Dihydro-2-fluoro-deschloroketamine were determined and then were synthesized specifically.The structures were identified by 1H NMR,13C NMR and 2D NOE NMR.The HPLC-QQQ MS/MS method for the detection of 2-fluoro-deschloroketamine,nor-2-fluoro-deschloroketamine,cis-Dihydro-2-fluoro-deschloroketamine and trans-Dihydro-2-fluoro-deschloroketamine in urine was established,which possesses a good linear relationship for 2-fluoro-deschloroketamine and its three main metabolites at the concentration range of 0.5～200 ng/mL,with the linear correlation coefficients all greater than 0.996 3,and the recoveries ranging from 81.60％to 119.33％.The quantitation of 2-fluoro-deschloroketamine and its three metabolites in actual urine samples was detected by the established method.This study determined the specific structures of two first-phase metabolites of 2-fluoro-deschloroketamine.The developed testing method has low detection limit,high recovery,and good reproducibility,which can be used in the qualitative and quantitative detection for the stable metabolites of 2-fluoro-deschloroketamine.
关键词
法医毒物学/氟胺酮/核磁/顺式氟胺醇/反式氟胺醇/高效液相色谱-三重四极杆串联质谱Key words
forensic toxicology/2-fluoro-deschloroketamine/nuclear magnetic resonance(NMR)/cis-Dihydro-2-fluoro-deschloroketamine/trans-Dihydro-2-fluoro-deschloroketamine/high performance liquid chromatography-triple quadrupole mass spectrometry引用本文复制引用
基金项目
国家自然科学基金青年科学基金(22104149)
出版年
2024
国家科技期刊平台
NSTL
万方数据