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.
目的: 建立基于傅里叶变换红外光谱（Fourier transform infrared spectroscopy，FTIR）、气相色谱-四极杆飞行时间质谱（gas chromatography-quadrupole time-of-flight mass spectrometry，GC-QTOF-MS）、超高效液相色谱-线性离子阱-四极杆-轨道阱质谱（ultra-high performance liquid chromatography-linear ion trap quadrupole-orbitrap mass spectrometry，UPLC-LTQ-Orbitrap MS）和核磁共振氢谱（1H-nuclear magnetic resonance spectroscopy，1H-NMR）技术联合鉴定未知样品的方法。方法: 采用傅里叶变换红外光谱仪直接检测未知样品；未知样品用含内标SKF525A的甲醇溶液溶解，上清液供GC-QTOF-MS和UPLC-LTQ-Orbitrap MS检测；未知样品用氘代甲醇溶液溶解后供1H-NMR检测。结果: 未知样品获得的红外光谱特征吸收峰为1 682（C=O 键）、1 503、1 488、1 436、1 363、1 256、1 092、1 035、935、840和800 cm-1，GC-QTOF-MS特征碎片离子m/z为86.096 4（基峰）、58.065 1、149.023 5、121.028 6和65.038 6，UPLC-LTQ-Orbitrap MS测得的精确质量数[M+H]+为236.127 7。样品经1H-NMR分析，鉴定为合成卡西酮类新精神活性物质Eutylone。结论: 本研究建立的方法可用于Eutylone的结构确证。.
Keywords: 1 H-nuclear magnetic resonance spectroscopy (1 H-NMR); Eutylone; Fourier transform infrared spectroscopy (FTIR); forensic toxicological analysis; gas chromatography-quadrupole time-of-flight mass spectro-metry (GC-QTOF-MS); new psychoactive substance; synthetic cathinones; ultra-high performance liquid chromatography-linear ion trap quadrupole-orbitrap mass spectrometry (UPLC-LTQ-Orbitrap MS).