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

作　　者：杨乔 吴法丞 沈昕怡 章健 丁伟光 吴波[1,2] Yang Qiao;Wu Facheng;Shen Xinyi;Zhang Jian;Ding Weiguang;Wu Bo(Narcotic Control Division of Nanjing Public Security Bureau,Nanjing 210042,China;School of Pharmacy,China Pharmaceutical University,Nanjing 210009,China)

机构地区：[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

出　　处：《中国法医学杂志》2024年第1期62-67,共6页Chinese Journal of Forensic Medicine

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(QTRAP LC-MS/MS)的检测方法。方法将洗净晾干的20 mg头发加入1 mL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0.01~2.00ng/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%。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。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.Afer 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 coeficients 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,eficient,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 

分 类 号：D918.93[政治法律—法学]