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作 者:邸玉敏[1,2] 肖楠 王瑞花[4] 周欣欣 阮世超[1] 马华 常靖[4] 张景然 Di Yumin;Xiao Nan;Wang Ruihua;Zhou Xinxin;Ruan Shichao;Ma Hua;Chang Jing;Zhang Jingran(Narcotics Control Bureau of Tianjin Public Security Bureau,Tianjin 300380,China;Tianjin Public Security Profession College,Tianjin 300000,China;Institute of Forensic Science Tianjin Public Security Bureau,Tianjin,300380,China;Institute of Forensic Sciences Ministry of Public Security P.R.C.,Bejjing 100038,China;SCIEX,Shanghai 200050,China)
机构地区:[1]天津市公安局禁毒总队,天津300380 [2]天津公安警官职业学院,天津300000 [3]天津市公安局物证鉴定中心,天津300380 [4]公安部鉴定中心,北京100038 [5]上海爱博才思分析仪器贸易有限公司,上海200050
出 处:《中国法医学杂志》2022年第6期575-578,583,共5页Chinese Journal of Forensic Medicine
基 金:公安部技术研究计划重点项目(2021JSZ05);公安部鉴定中心基本科研业务项目(2021JB007)。
摘 要:目的 建立准确、快速鉴定血液中7种国内常见新型合成大麻素(ADB-BUTINACA、ADB-4enPINACA、JWH-122、MDMB-4en-PINACA、4CN-CUMYL-BUTINACA、4F-MDMB-BUTINACA、5F-EMB-PICA)的液相色谱-四级杆/线性离子阱质谱(QTRAP LC-MSMS)检测方法。方法 全血样品经乙腈提取后高速离心取上清液,以含有0.1%甲酸的水溶液和0.1%甲酸的乙腈作为流动相,选用Phenomenex Kinetex?C18(100×2.1 mm,2.6μm)色谱柱分离,采用多反应监测触发增强子离子扫描(MRM-IDA-EPI),结合7种合成大麻素的EPI谱库检索的多种模式进行分析。结果 7种合成大麻素在1.0~200.0 ng/mL范围内线性关系良好,线性相关系数> 0.995;血中方法检出限(S/N≥3)为0.1~0.5 ng/mL,定量检测限均为1.0 ng/mL,在5.0、50.0、100.0 ng/mL低中高水平添加血样回收率为80.1%~110.3%,相对标准偏差均小于10%。结论 本方法简便、快捷、可靠、灵敏度高,可满足合成大麻素滥用者血液的定性定量分析。Objective To develop a method for determination of 7 kinds of synthetic cannabinoids(ADB-BUTINACA,ADB-4en-PINACA, JWH-122, MDMB-4en-PINACA,4CN-CUMYL-BUTINACA,4F-MDMB-BUTINACA and 5F-EMBPICA) in blood by using high performance liquid chromatography-tandem hybrid triple-quadrupole linear ion trap mass spectrometry(QTRAP LC-MS/MS). Methods The supernatant of blood samples were purified with membrane after extracted by methanol/acetonitrile(v/v,1/1) and centrifuged, then separated on a Phenomenex Kinetex?C18(100 × 2.1mm, 2.6 μm), which was eluted by the mobile phase of 0.1 % formic acid and 0.1 % formic acid/acetonitrile. A multiple reaction monitoring(MRM) as survey scan and an enhanced product ion(EPI) scan as dependent scan were performed in an information dependent acquisition(IDA) experiment. Results The linearity of synthetic cannabinoids were pretty good when the concentration was from 1.0 ~ 2 00.0ng/mL. The correlation coefficients were all above 0.995. The limits of detection(LODs, S/N≥ 3) were 0.1 ~ 0.5 ng/mL, and the limits of quantitative detection(LOQs, S/N≥ 10) were 1.0 ng/mL.The mean recovery rate at 5.0、5.0、100.0 ng/mL were 80.1 % ~ 110.3 %, and the RSD were < 10 %. Conclusion The established method is simple, rapid, sensitive and with high reliability, and is appropriate for the identification.
关 键 词:合成大麻素 血液 液相色谱-四级杆/线性离子阱质谱 快速检测 方法学
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