Many new psychoactive substances(NPSs)with different chemical structures have emerged in the illicit drug market in the last decade.The present work was aimed at the development of a simple method in gas chromatograph...Many new psychoactive substances(NPSs)with different chemical structures have emerged in the illicit drug market in the last decade.The present work was aimed at the development of a simple method in gas chromatography/mass spectrometry(MS)for the determination of NPS of different classes,the use of cannabinoids,and,at the same time,the evaluation of methadone therapy in hair matrix,within our routine analysis control for methadone treatment or from autopsy cases.The determination of synthetic cannabinoids and methadone therapy used an extraction method based on incubation in concentrated sodium hydroxide(NaOH)solution,providing a dissolution of the keratin matrix.The described method was applied on 15 authentic specimens from our cases:five showed the presence of methadone and 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine(EDDP).The described method can be useful not only in the forensic investigation of NPS-related addiction histories but also in epidemiological and retrospective studies on the spread of NPS among specific safety-sensitive social workers.The GC instrument was an Agilent 7820A(Agilent Technologies,Santa Clara,CA,USA),and the detection system was an Agilent 5977B single quadrupole MS operating in selective ion monitoring mode.Wlidation parameters such as limit of detections(LODs),limit of quantifications(LOQs),repeatability,accuracy,and linearity were satisfactory for its application on real specimens.LODs,LOQs,2?2,%CY standard deviation,and the mean concentration for the analyzed compounds are reported in Table lb.Accuracy and repeatability were acceptable for all the analytes at their respective LOQs.Recovery experiments varied from 58.3%to 103.0%,thus allowing the application on authentic specimens.The described method can be useful not only in the forensic investigation ofNPS-related addiction histories but also in epidemiological and retrospective studies on the spread of NPS among specific safety-sensitive social workers,such as drivers.展开更多
目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-py...目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。展开更多
文摘Many new psychoactive substances(NPSs)with different chemical structures have emerged in the illicit drug market in the last decade.The present work was aimed at the development of a simple method in gas chromatography/mass spectrometry(MS)for the determination of NPS of different classes,the use of cannabinoids,and,at the same time,the evaluation of methadone therapy in hair matrix,within our routine analysis control for methadone treatment or from autopsy cases.The determination of synthetic cannabinoids and methadone therapy used an extraction method based on incubation in concentrated sodium hydroxide(NaOH)solution,providing a dissolution of the keratin matrix.The described method was applied on 15 authentic specimens from our cases:five showed the presence of methadone and 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine(EDDP).The described method can be useful not only in the forensic investigation of NPS-related addiction histories but also in epidemiological and retrospective studies on the spread of NPS among specific safety-sensitive social workers.The GC instrument was an Agilent 7820A(Agilent Technologies,Santa Clara,CA,USA),and the detection system was an Agilent 5977B single quadrupole MS operating in selective ion monitoring mode.Wlidation parameters such as limit of detections(LODs),limit of quantifications(LOQs),repeatability,accuracy,and linearity were satisfactory for its application on real specimens.LODs,LOQs,2?2,%CY standard deviation,and the mean concentration for the analyzed compounds are reported in Table lb.Accuracy and repeatability were acceptable for all the analytes at their respective LOQs.Recovery experiments varied from 58.3%to 103.0%,thus allowing the application on authentic specimens.The described method can be useful not only in the forensic investigation ofNPS-related addiction histories but also in epidemiological and retrospective studies on the spread of NPS among specific safety-sensitive social workers,such as drivers.
文摘目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。
