高分辨质谱法和核磁共振法定性分析合成阿片类新精神活性物质2-甲基-布桂嗪

Qualitative Analysis of A Synthetic Opioid New Psychoactive Substance 2-Methyl-Bucinnazine by High Resolution Mass Spectrometry and Nuclear Magnetic Resonance

利用气相色谱-四极杆飞行时间质谱法(GC-Q-TOF MS)、高效液相色谱-线性离子阱/静电场轨道阱质谱法(HPLC-LTQ/Orbitrap MS)和核磁共振法(NMR)对缴获的未知样品进行定性分析。样品经甲醇溶解,涡旋、离心,取上清液供GC-Q-TOF MS检测,保留时间为27.92 min组分的质谱碎片主要特征离子质荷比(m/z)为286.203 7,215.154 0,195.149 0,172.111 8,117.069 6(基峰)。经HPLC-LTQ/Orbitrap MS分析,质子化分子离子m/z为287.212 1。对比国家管制麻醉药品布桂嗪的相应质谱信息[主要特征离子m/z为272.188 1,201.138 4,181.133 3,172.111 8,117.069 6(基峰),质子化分子离子m/z为273.196 5],推测未知样品为布桂嗪的甲基衍生物,分子式为C_(18)H_(26)N_(2)O。经NMR分析,确认该未知样品为合成阿片类新精神活性物质2-甲基-布桂嗪。

Gas chromatography-quadrupole time-of-flight mass spectrometry(GC-Q-TOF MS), high performance liquid chromatography-linear ion trap/orbitrap mass spectrometry(HPLC-LTQ/Orbitrap MS) and nuclear magnetic resonance(NMR) were used to qualitative analysis the captured unknown sample. The sample was dissolved in methanol. After vortex and centrifugation, the supernatant was used for GC-Q-TOF MS detection. The values of mass-to-charge ratio(m/z) of main characteristic fragment ions showed by the component with retention time of 27.92 min were 286.203 7, 215.154 0, 195.149 0, 172.111 8, 117.069 6(base peak). HPLC-LTQ/Orbitrap MS analysis showed that the protonated molecular ion was m/z 287.212 1. The corresponding MS information of the national controlled narcotic drug bucinnazine with the main characteristic fragment ions of m/z 272.188 1, 201.138 4, 181.133 3, 172.111 8, 117.069 6(base peak) and the protonated molecular ion of m/z 273.196 5 were compared. The unknown sample was inferred as methyl derivative of bucinnazine, and its molecular formula was C_(18)H_(26)N_(2)O. After NMR analysis, the unknown sample was confirmed as the new opioid psychoactive substance 2-methyl-bucinnazine.