超高效液相色谱—串联质谱法检测毛发中2-邻氟苯基-2-乙氨基环己酮  

Determination of 2-o-fluorophenyl-2-ethylaminocyclohexanone in Human Hair by HPLC/MS/MS

作　　者：祁观 仇文璞 柴一麟 白登文 杨淑颐 龙娇 罗莉娅 杨丽 Qi Guan;Chou Wenpu;Chai Yilin;Bai Dengwen;Yang Shuyi;Long Jiao;Luo Liya;Yang Li(Sichuan Provincial Technical Center for Drug Monitoring(Sichuan Branch of the State Drug Laboratory),Chengdu 610000,China)

机构地区：[1]四川省毒品监测技术中心(国家毒品实验室四川分中心),四川成都610000

出　　处：《广东化工》2025年第3期121-124,共4页Guangdong Chemical Industry

摘　　要：目的:建立在毛发样本中精准测定2-邻氟苯基-2-乙氨基环己酮的超高效液相—串联质谱检测方法。方法:毛发样品经1 mL甲醇提取液破碎溶解,经0.22μm滤膜过滤后,采用ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm)色谱柱,以含0.1%甲酸的乙腈—水为流动相进行梯度洗脱,流速0.4 mL/min。质谱的检测采用电喷雾电离-正离子、动态MRM的检测模式。结果:该方法实现了对2-邻氟苯基-2-乙氨基环己酮的定性、定量分析,目标物在0.1 ng/mL~100 ng/mL范围内具有良好的线性关系,R^(2)大于0.997,检出限为10 pg/mL,定量限为100 pg/mL,不同浓度添加样品的提取回收率在92.31%~95.49%范围内,基质效应在106.14%~130.17%范围内,日内、日间RSD均小于10%。结论:该方法具有快速、灵敏、准确、稳定、操作简便等优势,能够满足部分胺酮类物质在毛发中定性、定量分析的要求,可以为相关案件中胺酮类新精神活性物质的检验鉴定提供借鉴,为推动2-邻氟苯基-2-乙氨基环己酮的列管提供参考。Objective:establish an liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for accurate determination of 2-o-fluorophenyl-2-ethylaminocyclohexanone in hair samples.Methods:The hair samples were broken and dissolved by 1 mL methanol extract,filtered by 0.22μm filter membrane,and then used ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm)chromatographic column,acetonitrile-water containing 0.1%formic acid was used as mobile phase for gradient elution at a flow rate of 0.4 mL/min.The detection mode of mass spectrometry was electrospray ionization-positive ion and dynamic MRM.Results:The method realizes the qualitative and quantitative analysis determination of 2-o-fluorophenyl-2-ethylaminocyclohexanone.The linear relationship of the target was good in the range of 0.1 ng/mL~100 ng/mL,and R^(2) was greater than 0.997,detection limit was 10 pg/mL,quantitative limit was 100 pg/mL,and the recovery of the added samples was in the range of 92.31.6%~95.49%,The matrix effect ranged from 106.14%to 130.17%,and the intra-day and inter-day RSDs were less than 10%.Conclusion:the method is rapid,sensitive,accurate,stable and easy to operate.It can meet the requirements of qualitative and quantitative analysis determination of some ketones in human hair,it can provide reference for the identification of new psychoactive substances of ketones in relevant cases and promote the enantioseparation of 2-o-fluorophenyl-2-ethylaminocyclohexanone.

关 键 词：新精神活性物质 胺酮类物质 毛发检测 超高效液相色谱-串联质谱 

分 类 号：TQ[化学工程]