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作 者:何思阳[1] 龚飞君 袁晓亮 盛振海 徐金伦 郑水庆[1] 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)
机构地区:[1]上海市公安局物证鉴定中心,上海200083 [2]上海市刑事科学技术研究院,上海200083
出 处:《分析试验室》2020年第8期947-952,共6页Chinese Journal of Analysis Laboratory
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.
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