摘要
建立了采用红外光谱(FTIR)、气相色谱-四级杆飞行时间质谱(GC/Q-TOF)和液相色谱-高分辨质谱(UPLC-LTQ-Orbitrap)鉴定检材中氯硝唑仑的方法,并通过核磁共振氢谱(1HNMR)进行确认。样品经FTIR检测在1512cm^-1和1351cm^-1处存在芳香族硝基红外光谱特征吸收峰。用甲醇溶解后,上清液经GC/Q-TOF检测,保留时间为18.82 min组分的质谱碎片主要特征离子峰有353.0680(分子离子峰),324.0534(基峰),278.0605,249.0659,203.0730等。经UPLC-LTQ-Orbitrap检测,保留时间为12.72 min的质子化分子离子m/z为354.0739,碰撞诱导解离(CID)模式下二级质谱主要离子有326.0564,319.1063,308.0822。经SWGDRUG3.3谱库检索,资料对比和核磁共振氢谱共同确认目标物为苯二氮[艹卓][艹卓]类新精神活性物质氯硝唑仑。
A method was developed for the identification of clonazolam in sample by FTIR,GC/Q-TOF and UPLC-LTQ-Orbitrap,then the sample was confirmed by 1 HNMR.FTIR spectrum had characteristic absorption peaks at 1512 and 1351 cm^-1(Ar-NO2).The supernatant was subjected and analyzed by GC/Q-TOF after samples were dissolved in methanol.Component(tR=18.82 min)showed characteristic fragment ion peaks at m/z 353.0680(molecular ion peak),324.0534(base peak),278.0605,249.0659 and 203.0730,etc.It was also detected by UPLC-LTQ-Orbitrap(tR=12.72 min),appearing its protonated molecular ion peak m/z 354.0739 and m/z 326.0564,319.1063 and 308.0822 in CID MS/MS,respectively.The sample was identified as a designer benzodiazepine clonazolam according to the search in SWGDRUG3.3 library,and the comparison with literature data and the 1H NMR detection.
作者
何思阳
龚飞君
袁晓亮
盛振海
徐金伦
郑水庆
HE Siyang;GONG Feijun;YUAN Xiaoliang;SHENG Zhenhai;XU Jinlun;ZHENG Shuiqing(Institute of Forensic Science of Shanghai Public Security Bureau,Shanghai 200083;Shanghai Research Institute of Criminal Science and Technology,Shanghai 200083)
出处
《分析试验室》
CAS
CSCD
北大核心
2020年第8期947-952,共6页
Chinese Journal of Analysis Laboratory
作者简介
何思阳,男,(1988-)程师。研究方向:毒品毒物检验鉴定,xhesy@foxmail.com;通信作者:郑水庆,男(1973-),高级工程师。研究方向:毒品毒物检验鉴定,shuiqingzheng@sina.com。
