人体毛发中氯胺酮及其代谢物的超高效液相色谱-串联质谱法检验及含量统计分析  

Determination and Statistical Analysis of Ketamine and Its Metabolites in Human Hair by Ultra-performance Liquid Chromatography Coupled with Mass Spectrometry

作　　者：侯伟 张蕾萍[2] 王继芬[1] 魏春明[2] 卢亮 仲利静[2] 刘浩田 HOU Wei;ZHANG Lei-ping;WANG Ji-fen;WEI Chun-ming;LU Liang;ZHONG Li-jing;LIU Hao-tian(School of Investigation,People's Public Security University of China,Beijing 100038,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]公安部物证鉴定中心,北京100038

出　　处：《分析测试学报》2021年第10期1453-1459,1466,共8页Journal of Instrumental Analysis

基　　金：中央级公益性科研院所基本科研业务费专项资金项目(2019JB031)。

摘　　要：建立了一种高动能研磨结合超高效液相色谱-串联质谱(UPLC-MS/MS)快速检验毛发中氯胺酮及其代谢物的方法,并考察了清洗程序和提取方法对氯胺酮及其代谢物检出效果的影响。确定最佳实验方法为:50 mg头发经0.1%十二烷基硫酸钠、超纯水和丙酮清洗2次后取20 mg置于专用研磨管内,加入1 mL甲醇,使用球磨仪以3000 r/min研磨3 min,超声2 h,离心过膜进样。结果显示:毛发中氯胺酮、去甲氯胺酮和羟基去甲氯胺酮含量分别在0.01~5.0、0.01~5.0、0.05~5.0 ng/mg范围内线性关系良好,相关系数(r)均大于0.99,回收率为86.7%~106%,基质效应为88.1%~99.6%,日内及日间精密度分别为0.72%~4.1%和1.9%~6.3%。采用该方法检测了50份实际毛发样本,并对氯胺酮、去甲氯胺酮和羟基去甲氯胺酮在阳性毛发中的含量数据进行统计,分析了毛发中氯胺酮及其两种主要代谢物的含量分布情况及原药与代谢物的含量关系,50份真实毛发样本中氯胺酮的最低含量为0.30 ng/mg,羟基去甲氯胺酮与氯胺酮的含量相近且去甲氯胺酮与氯胺酮之间的含量比率为0.05~0.60。该研究结果可为禁毒人员处理涉毒案件提供理论支撑与方法参考。An ultra-performance liquid chromatography-mass spectrometry(UPLC-MS/MS)with high kinetic energy grinding was established for the rapid detection of ketamine and its metabolites in hair.The effects of cleaning procedures and extraction methods on the detection of ketamine and its metabolites were investigated,respectively,and the best experimental scheme was determined.50 mg hair was washed twice with 0.1%sodium lauryl sulphate,ultrapure water and acetone.Then 20 mg of the washed hair and 1 mL methanol were placed in a special grinding bottle,and mixed in an oscillating manner.The hair was ground for 3 min at a frequency of 3000 r/min by the grinding machine.The grinding fluid was ultrasonically disposed for 2 hours,then detected after centrifuga⁃tion and filtration.There were good linear relationships for contents of ketamine,norketamine and hydroxynorketamine in hair in the range of 0.01-5.0,0.01-5.0,0.05-5.0 ng/mg,with their correlation coefficients higher than 0.99.The extraction recoveries ranged from 86.7%to 106%,and the matrix effects were between 88.1%and 99.6%for all the analytes.The intra-day and inter-day precisions were in the range of 0.72%-4.1%and 1.9%-6.3%,respectively.Meanwhile,50 hair samples of drug addicts were tested in this way.The content data of ketamine,norketamine and droxynorketamine in positive hair were obtained and analyzed.The content distribution of ketamine and its metabolites and the relationship between the contents of ketamine and its metabolites in hair were determined by data analysis.The minimum content of ketamine was 0.30 ng/mg.The content of droxynorketamine was similar to ketamine while the content ratio between norketamine and ket⁃amine ranged from 0.05 to 0.60.These analyses and conclusions could provide a theoretical support and a method reference for the drug-related cases.

关 键 词：毛发 超高效液相色谱-串联质谱 氯胺酮及其代谢物 含量统计 

分 类 号：O657.7[理学—分析化学]