盐酸氟胺酮的结构确证和核磁共振定量分析  

Structural Confi rmation and Quantitative Nuclear Magnetic Resonance Analysis into 2-Fluoro-deschloroketamine Hydrochloride

作　　者：吴波 郄一奇[1] 杨乔 田冰冰 赵钰馨 苏梦翔 狄斌 WU Bo;QIE Yiqi;YANG Qiao;TIAN Bingbing;ZHAO Yuxin;SU Mengxiang;DI Bin(Department of Pharmaceutical Analysis,College of Pharmacy,China Pharmaceutical University,Nanjing 211198,China;Narcotic Control Division of Nanjing Public Security Bureau,Nanjing 210042,China;China National Narcotics Control Commission-China Pharmaceutical University Joint Laboratory on Key Technologies of Narcotics Control,Nanjing 210009,China)

机构地区：[1]中国药科大学药学院药物分析系,南京211198 [2]南京市公安局禁毒支队,南京210042 [3]国家禁毒委员会办公室–中国药科大学禁毒关键技术联合实验室,南京210009

出　　处：《刑事技术》2023年第3期262-267,共6页Forensic Science and Technology

基　　金：国家自然科学基金(81872833)。

摘　　要：对氟胺酮缴获物进行结构确证和含量测定。利用元素分析、紫外吸收光谱(UV)、红外吸收光谱(IR)、高分辨质谱(QTOF/MS)、核磁共振谱(1H NMR、13C NMR、DEPT、1H-1H COSY、1H-13C HMBC、1H-13C HSQC)等手段进行定性分析;建立定量核磁共振氢谱法(1H-qNMR)进行定量分析,以富马酸为内标,以0.5mL氘代二甲亚砜和0.1 mL重水混合溶液为溶剂,激发脉冲角度为30°,测定温度为303 K,脉冲延迟时间为30 s,采样次数为16次。实验确证了缴获物为盐酸氟胺酮,并成功建立了定量核磁共振法,此方法专属性良好;稳定性可达56 h;耐用性符合要求;盐酸氟胺酮与内标富马酸的质子摩尔比在0.453 0~2.151 2范围内线性关系良好,R2为1.000;缴获物中盐酸氟胺酮的含量测定结果为99.86%。定量核磁共振法操作简单、快速,在无对照品或对照品难以获得的情况下,可直接用于氟胺酮的定量检测,可为苯环利定类物质的分析提供参考。2-Fluoro-deschloroketamine(2-FDCK),a new substitute for ketamine undergone into changing halogenated element and a new psychoactive substance of phencyclidine class that is being widely abused,has been presently paid of its main research on the analysis of suspected seizures and biological samples.In terms of qualitative determination about 2-FDCK,there are publications relating to the data from IR,mass spectrometry(MS)and NMR(1H NMR,13C NMR,19F NMR).2-FDCK’s quantitative detection primarily adopts gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry,yet leaving it prone to be influenced with the factors of difficulty in obtaining the reference substance and high price.In this paper,one seizure was to identify whether it harbors 2-FDCK via the measures of confirmation of evidential structure and determination of the content of the 2-FDCK hydrochloride,with the qualitative analysis being carried out by elemental analysis,ultraviolet absorption spectrometry(UV),infrared absorption spectrometry(IR),time offlight mass spectrometry(TOF/MS)and nuclear magnetic resonance spectrometry(1H NMR,13C NMR,DEPT,1H-1H COSY,1H-13C HMBC,1H-13C HSQC).Meanwhile,a 1H quantitative NMR(1H-qNMR)method was hence established and validated for determination of the seized 2-FDCK hydrochloride.For the method,the sample solution was prepared with fumaric acid as the internal standard and the mixture of 0.5 mL DMSO-d6 plus 0.1 mL D2O as the solvent.The NMR spectra were recorded through a standard pulse sequence at a pulse width of 30°.The determination temperature was set at 303 K.The relaxation delay time and the number of scans were optimized to 30 s and 16 times,respectively.The results showed that the accurate mass-to-charge(m/z)of the compound was 222.1283 under positive electrospray ionization,with the element analysis revealing the percentage content of C,H and N elements as the respective 60.24%,6.15%and 5.51%.The UV spectrums indicated the absorption peaks at 270 nm and 263 nm corresponded to the B ban

关 键 词：盐酸氟胺酮 结构鉴定 定量核磁共振 含量测定 

分 类 号：O657.2[理学—分析化学] D919.1[理学—化学]