摘要
目的建立基于傅里叶变换红外光谱(FTIR)、气相色谱-质谱联用(GC-MS)和核磁共振波谱技术联合鉴定未知样品的方法。方法未知样品采用红外衰减全反射ATR专用采样器直接检测;样品用含4-甲基甲卡西酮(4-MMC,内标物)的甲醇溶液溶解后经GC-MS检测;样品经氘代甲醇溶解后进行核磁氢谱(1H NMR)和碳谱(13C NMR)的检测。结果未知样品的红外光谱特征吸收峰主要为1 688,1 606,1 459,1 440,1 385,1 306,1 241,1 190,1 128,1 106,1 038,976,851,832,799,752,737,684 cm-1,获得的质谱特征碎片峰(m/z)为72.1(基峰),44.1,91.1,119.0,146.0,与美国禁毒署提供的相关谱库比对一致;用1H和13C NMR谱图对其结构进行了进一步的确证,认定未知样品为4-甲基乙卡西酮(4-MEC)。结论建立的未知物鉴定方法可用于新型策划毒品的定性鉴定。
Objective To establish methods for the identification of 4-methyl-N-ethylcathinone（4-MEC） by FTIR, GC-MS and NMR techniques. Method The suspicious unknown samples were analyzed by FTIR and GC-MS. 4-MMC was used as the internal standard. The analytes were diluted in CD3 OD for the identification of structure using1 H and13C NMR. Results The infrared spectrum of 4-MEC has characteristic absorption peaks at 1688, 1606, 1459, 1440, 1385, 1306, 1241, 1190, 1128,1106, 1038, 976, 851, 832, 799, 752, 737 and 684 cm-1. The mass fragment ion peaks（m/z） are 72.1（base）, 44.1, 91.1, 119.0and146.0. The results are consistent with the information in the U.S. Drug Enforcement Administration spectra library. Further confirmed by1 H and13C NMR spectrum, the sample was identified as the new designer drug 4-MEC. Conclusion The method is suitable for the identification of new designer drugs.
出处
《中国司法鉴定》
2015年第3期43-46,共4页
Chinese Journal of Forensic Sciences
基金
上海市刑事科学技术研究院重点实验室自立课题项目资助(2014XCWZZ02)
