1、法 医 学 杂 志 2022年 10月 第38卷 第5期电子烟油和毛发中合成大麻素 CUMYL-PEGACLONE的检测焦台风,李亚庆,康刚,陈深树,程良红广东南天司法鉴定所,广东 深圳 518003摘要:目的 建立联合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)和气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)检测电子烟油和毛发中合成大麻素 5-戊基-2-(2-苯基丙-2-基)-2,5-二氢-1H-吡啶4,
2、3-b吲哚-1-酮(CUMYL-PEGACLONE)的方法。方法 采用 HPLC-MS/MS 和 GC-MS 建立 CUMYL-PEGACLONE 检测方法,对涉毒人员毛发和查获的电子烟油进行检测。结果 GC-MS测得CUMYL-PEGACLONE主要质谱特征离子m/z为91、179、197、254和372;CUMYL-PEGACLONE在250 ng/mL质量浓度范围内线性关系良好,线性相关系数(r)大于 0.99;毛发中 CUMYL-PEGACLONE 的 HPLC-MS/MS 方法检出限为 0.01 ng/mg,定量限为0.02 ng/mg;电子烟油中CUMYL-PEGACLONE的HP
3、LC-MS/MS方法检出限为1 ng/mg,定量限为2 ng/mg;CUMYL-PEGACLONE 在空白毛发和电子烟油基质中高、中、低 3 个添加浓度下的回收率分别为 98.2%132.4%和 93.5%110.6%,日内精密度和日间精密度分别为 1.2%12.9%和 0.7%2.9%。专案中 15例涉毒人员头发中均检出CUMYL-PEGACLONE,除1例低于定量限,另14例人员头发中CUMYL-PEGACLONE质量分数为0.0350.563 ng/mg;2份电子烟油中CUMYL-PEGACLONE的质量分数分别为0.17%和0.21%。结论 建立的HPLC-MS/MS和GC-MS方法应
4、用于涉毒专案中CUMYL-PEGACLONE的检测,为办案机关快速侦办涉毒专案提供了有力证据支撑,亦为今后涉及此类物质的鉴定提供参考依据。关键词:法医毒物化学;合成大麻素;高效液相色谱-串联质谱法;气相色谱-质谱法;5-戊基-2-(2-苯基丙-2-基)-2,5-二氢-1H-吡啶4,3-b吲哚-1-酮中图分类号:DF795.1 文献标志码:A doi:10.12116/j.issn.1004-5619.2022.320701文章编号:1004-5619(2022)05-0595-06Detection of Synthetic Cannabinoid CUMYL-PEGACLONE in E-C
5、igarette Oil and HairJIAO Tai-feng,LI Ya-qing,KANG Gang,CHEN Shen-shu,CHENG Liang-hongGuangdong Nantian Institute of Forensic Science,Shenzhen 518003,Guangdong Province,ChinaAbstract:Objective To establish a combined high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)and gas
6、chromatography-mass spectrometry(GC-MS)method to detect the synthetic cannabinoid CUMYL-PEGACLONE in e-cigarette oil and hair.Methods HPLC-MS/MS and GC-MS were used to establish the detection method of CUMYL-PEGACLONE,and the hair of drug-involved persons and the seized e-cigarette oil were detected
7、.Results The main mass spectrometry characteristic ions m/z of CUMYL-PEGACLONE measured by GC-MS were 91,179,197,254 and 372.CUMYL-PEGACLONE had a good linear relationship in the mass concentration range of 2-50 ng/mL,and the linear correlation coefficient(r)was greater than 0.99.The limit of detect
8、ion(LOD)of CUMYL-PEGACLONE in hair was 0.01 ng/mg,and the limit of quantitation(LOQ)was 0.02 ng/mg.The LOD of CUMYL-PEGACLONE in e-cigarette oil was 1 ng/mg,and the LOQ was 2 ng/mg.The average recoveries of CUMYL-PEGACLONE under the attempt at high,intermediate and low levels in blank human hair and
9、 e-cigarette oil matrix were 98.2%-132.4%and 93.5%-110.6%,and the intraday and intraday precision were 1.2%-12.9%and 0.7%-2.9%.CUMYL-PEGACLONE was detected in the hair of 15 drug-involved persons.Except for 1 person who was lower than LOQ,the concentration of CUMYL-PEGACLONE in the hair of other 14
10、persons was 0.035-0.563 ng/mg.The mass fraction of CUMYL-PEGACLONE in 2 e-cigarette oil were 0.17%and 0.21%,respectively.Conclusion The established HPLC-MS/MS and GC-MS methods are applied to the detection of HPLC-MS/MS in drug-related cases,which provides strong evidence support for the handling au
11、thority to quickly investigate these cases,and also provides a reference for the identification of such substances in future.Keywords:forensic toxicology;synthetic cannabinoid;high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS);gas chromatography-mass spectrometry(GC-MS);CUMY
12、L-PEGACLONE 论著 基金项目:深圳市科技创新委员会资助项目(JSGG20210802152810032)作者简介:焦台风(1986),女,主检法医师,主要从事体内外毒(药)物的检验鉴定;E-mail:通信作者:程良红,男,主任技师,主要从事体内外毒(药)物的检验鉴定;E-mail:引用格式:焦台风,李亚庆,康刚,等.电子烟油和毛发中合成大麻素 CUMYL-PEGACLONE 的检测J.法医学杂志,2022,38(5):595-600.To cite:JIAO T F,LI Y Q,KANG G,et al.Detection of synthetic cannabinoid CUMY
13、L-PEGACLONE in e-cigarette oil and hairJ.Fayixue Zazhi,2022,38(5):595-600.595Journal of Forensic Medicine,October 2022,Vol.38,No.5近几年,我国禁毒部门持续推进专项行动,加之疫情影响,我国呈现吸毒人数减少、规模化制毒活动减少、国内缴毒总量减少的积极变化,冰毒、海洛因、氯胺酮等 3类主流毒品滥用治理成效显现。吸毒者为寻求替代品满足毒瘾,交叉滥用非惯用毒品形势日趋严峻1-3,其中以合成大麻素为代表的新精神活性物质(new psychoactive substance,NP
14、S)是这类非惯用毒品的典型代替物。合成大麻素类物质是一类人工合成物质,具有与四氢大麻酚(9-tetrahydrocannabinol,9-THC)类似的生理、药理作用和激动大麻素受体的能力,吸食后能产生和传统大麻同样甚至更强烈的欣快感4-6,由于合成大麻素类物质成本更低,更易获取,现已成为 NPS中涵盖物质种类最多、滥用最为严重的家族。自 2021 年 7 月 1 日我国将合成大麻素类物质整类列管以来,市面上贩卖和吸食含有合成大麻素电子烟油的情况虽有好转但仍屡见不鲜。国内已报道合成大麻素的检测方法主要有傅里叶变换红外光谱法(Fourier transform infrared spectros
15、copy,FTIR)7、气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)8、液 相 色 谱-质 谱 联 用 法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)9和超高效液相色谱-四级杆-飞行时间质谱(ultra-high performance liquid chromatography series quadrupole time-of-flight mass spectrometry,UPLC-QTOF-MS)10等,对新出现的合成大麻素则大多是经制备液相分离后综合采用
16、 FTIR、GC-MS、核磁共振(nuclear magnetic resonance,NMR)等多技术联合进行结构剖析11-12。合成大麻素类 NPS 的鉴定是当前法医毒物实验室工作的重要需求,5-戊基-2-(2-苯基丙-2-基)-2,5-二氢-1H-吡啶4,3-b吲哚-1-酮(5-pentyl-2-(2-phenylpropan-2-yl)-2,5-dihydro-1H-pyrido4,3-b indol-1-one,CUMYL-PEGACLONE)属于吲哚类新型合成大麻素,是一种大麻素受体强效激动剂13-14,本研究旨在建立联合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)和GC-MS快速测定毛 发 和 电 子 烟 油 中 合 成 大 麻 素 CUMYL-PEGACLONE的方法,并应用于实际案例。1材料与方法1.1 主要仪器与试剂1290 Infinity II液相色谱-6470三重四极杆液质联 用 系 统(美 国 Agilent 公 司),7890