RESUMEN
OBJECTIVES: To establish a method to identify unknown sample based on the combined use of Fourier transform infrared spectroscopy (FTIR), gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS), ultra-high performance liquid chromatography-linear ion trap quadrupole-orbitrap mass spectrometry (UPLC-LTQ-Orbitrap MS) and 1H-nuclear magnetic resonance spectroscopy (1H-NMR) technique. METHODS: The unknown sample was directly analyzed by FTIR. The unknown sample was dissolved in methanol solution containing internal standard SKF525A and the supernatant was detected by GC-QTOF-MS and UPLC-LTQ-Orbitrap MS. The unknown sample was dissolved in methanol-d4 solution for structural analysis of 1H-NMR. RESULTS: The characteristic absorption peaks of FTIR spectra obtained from unknown sample were 1 682 (C=O bond), 1 503, 1 488, 1 436, 1 363, 1 256, 1 092, 1 035, 935, 840 and 800 cm-1, the characteristic fragment ions (m/z) of GC-QTOF-MS were 86.096 4 (base peak), 58.065 1, 149.023 5, 121.028 6 and 65.038 6, the accurate mass [M+H]+ detected by UPLC-LTQ-Orbitrap MS was 236.127 7. The sample was identified as synthetic cathinone new psychoactive substance Eutylone by 1H-NMR. CONCLUSIONS: The method established in this study can be used for structural confirmation of Eutylone.
Asunto(s)
Metanol , Cromatografía Líquida de Alta Presión/métodos , Espectrometría de Masas , Cromatografía de Gases y Espectrometría de Masas/métodos , Espectroscopía de Resonancia MagnéticaRESUMEN
The dopamine transporter (DAT) is the main target of methylphenidate (MPH), which remains the number one drug prescribed worldwide for the treatment of Attention-Deficit Hyperactivity Disorder (ADHD). In addition, abnormalities of the DAT have been widely associated with ADHD. Based on clinical and preclinical studies, the direction of DAT abnormalities in ADHD are, however, still unclear. Moreover, chronic treatment of MPH has been shown to increase brain DAT expression in both animals and ADHD patients, suggesting that findings of overexpressed levels of DAT in ADHD patients are possibly attributable to the effects of long-term MPH treatment rather than the pathology of the condition itself. In this chapter, we will discuss some of the effects exerted by MPH, which are related to its actions on catecholamine protein targets and brain metabolites, together with genes and proteins mediating neuronal plasticity. For this purpose, we present data from biochemical, proton nuclear magnetic resonance spectroscopy (1H-NMR) and gene/protein expression studies. Overall, results of the studies discussed in this chapter show that MPH has a complex biological/pharmacological action well beyond the DAT.
Asunto(s)
Trastorno por Déficit de Atención con Hiperactividad , Estimulantes del Sistema Nervioso Central , Metilfenidato , Animales , Trastorno por Déficit de Atención con Hiperactividad/tratamiento farmacológico , Encéfalo/metabolismo , Estimulantes del Sistema Nervioso Central/farmacología , Estimulantes del Sistema Nervioso Central/uso terapéutico , Proteínas de Transporte de Dopamina a través de la Membrana Plasmática/metabolismo , Metilfenidato/farmacología , Metilfenidato/uso terapéuticoRESUMEN
OBJECTIVES@#To establish a method to identify unknown sample based on the combined use of Fourier transform infrared spectroscopy (FTIR), gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS), ultra-high performance liquid chromatography-linear ion trap quadrupole-orbitrap mass spectrometry (UPLC-LTQ-Orbitrap MS) and 1H-nuclear magnetic resonance spectroscopy (1H-NMR) technique.@*METHODS@#The unknown sample was directly analyzed by FTIR. The unknown sample was dissolved in methanol solution containing internal standard SKF525A and the supernatant was detected by GC-QTOF-MS and UPLC-LTQ-Orbitrap MS. The unknown sample was dissolved in methanol-d4 solution for structural analysis of 1H-NMR.@*RESULTS@#The characteristic absorption peaks of FTIR spectra obtained from unknown sample were 1 682 (C=O bond), 1 503, 1 488, 1 436, 1 363, 1 256, 1 092, 1 035, 935, 840 and 800 cm-1, the characteristic fragment ions (m/z) of GC-QTOF-MS were 86.096 4 (base peak), 58.065 1, 149.023 5, 121.028 6 and 65.038 6, the accurate mass [M+H]+ detected by UPLC-LTQ-Orbitrap MS was 236.127 7. The sample was identified as synthetic cathinone new psychoactive substance Eutylone by 1H-NMR.@*CONCLUSIONS@#The method established in this study can be used for structural confirmation of Eutylone.