QTRAP LC-MS/MS方法分析头发中氯胺酮结构类似物
Detecting Ketamine analogues in hair samples by QTRAP LC-MS/MS
杨乔 1吴法丞 2沈昕怡 2章健 1丁伟光 1吴波3
作者信息
- 1. 南京市公安局禁毒支队,江苏南京 210042
- 2. 中国药科大学药学院,江苏南京 210009
- 3. 南京市公安局禁毒支队,江苏南京 210042;中国药科大学药学院,江苏南京 210009
- 折叠
摘要
目的 建立头发中氯胺酮结构类似物的液相色谱-四极杆/线性离子阱质谱(QTRAPLC-MS/MS)的检测方法.方法 将洗净晾干的20 mg头发加入1mL提取液冷冻研磨后冰浴超声提取,离心取上清液过滤膜后,经ACQUITY UPLC® HSS T3色谱柱分离,采用多反应监测模式同时测定10种氯胺酮结构类似物.以该方法分析20例阳性头发样本中乙基氟胺酮、去甲氟胺酮和替来他明的含量.结果 头发中10种氯胺酮结构类似物在0.01～2.00 ng/mg范围内线性关系良好,相关系数＞0.99,回收率为89.1％～106.1％,基质效应为88.3％～106.0％a 20例阳性头发样本中乙基氟胺酮的含量范围为0.02～8.35 ng/mg,平均值1.59 ng/mg,中位值0.40 ng/mg;去甲氟胺酮的含量范围为0.01～0.94 ng/mg,平均值0.28 ng/mg,中位值0.19 ng/mg;替来他明的含量范围为0.02～10.93 ng/mg,平均值2.69 ng/mg,中位值2.11 ng/mg.结论 本方法简便、高效、可靠,适用于头发中氯胺酮结构类似物的检验.样本数据为氯胺酮结构类似物的管控、鉴定提供了一定参考.
Abstract
Objective To develop a method for the determination of ketamine analogues in hair samples by liquid chromatography quadrupole linear ion trap mass spectrometry(QTRAP LC-MS/MS).Methods 20 mg of washed and dried hair was added to 1 mL extracting solution and then prepared using an ultrasonic extraction with frozen pulverization method.After centrifugation and purification with membrane,the supernatant was separated in a ACQUITY UPLC® HSS T3 column with gradient elution,finally tested with multiple reaction monitoring for the detection of 10 ketamine analogues.The above method was applied for quantitative analysis of ethylfluamine,F-norketamine and tiletamine in 20 positive samples.Results When the concentration ranged from 0.01 to 2.00 ng/mg,there was good linearity for 10 ketamine analogues with the correlation coefficients over 0.99.The recoveries ranged from 89.1％to 106.1％,and the matrix effects were between 88.3％and 106.0％.Among the 20 positive samples,the contents of ethylfluamine,F-norketamine and tiletamine in hair ranged between 0.02～8.35 ng/mg,0.01～0.94 ng/mg and 0.02～10.93 ng/mg,respectively.Their mean values were 1.59 ng/mg,0.28 ng/mg and 2.69 ng/mg.Their medians were 0.40 ng/mg,0.19 ng/mg and 2.11 ng/mg.Conclusion The established method was simple,efficient,reliable and suitable for the determination of ketamine analogues in hair.The data provided reference for the drug control and forensic science practice.
关键词
法医毒物学/头发/氯胺酮结构类似物/液相色谱-四极杆/线性离子阱质谱Key words
Forensic toxicology/Hair/Ketamine analogues/QTRAP LC-MS/MS引用本文复制引用
出版年
2024
NETL
NSTL
万方数据