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作 者:钱振华[1] 陈月猛 花镇东[3] QIAN Zhen-hua;CHEN Yue-meng;HUA Zhen-dong(Institute of Forensic Science Ministryof Public Security, Beijing 100038;Drug Control Unit of Guiyang Public Security Bureau ofGuizhou Province, Guiyang 550018;Drug Intelligence and Forensic Technology Center, Ministry of Public Security, Beijing 100193)
机构地区:[1]公安部物证鉴定中心,北京100038 [2]贵州省贵阳市公安局禁毒支队,贵阳550018 [3]公安部禁毒情报技术中心,北京100193
出 处:《分析试验室》2019年第3期270-274,共5页Chinese Journal of Analysis Laboratory
基 金:中央级公益性科研院所基本科研业务费专项资金(2017JB030)资助
摘 要:报道中国首次缴获的芬太尼类物质卡芬太尼,建立其气相色谱-质谱(GC-MS)、超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF MS)和红外光谱(FTIR)定性检验方法。未知样品用甲醇和水提取,取上清液,采用GC-MS和UPLC-Q-TOF MS进行分析;样品粉末置于衰减全反射(ATR)附件中,进行FTIR采集。GC-MS检测,保留时间为13. 05 min的未知组分的质谱碎片主要特征离子峰有m/z 303,105,243,187,96,154。UPLC-Q-TOF MS检测,保留时间为3. 976 min的未知组分的准分子离子峰为m/z 395. 2325,碰撞诱导解离(CID)模式下二级质谱主要离子有m/z 335. 2117,279. 1856,246. 1490,146. 0966,134. 0966,113. 0599。FTIR检测,在1724,1635,1593,1352,1225,704 cm-1等处出现吸收峰。经NIST谱库检索、已报道文献中信息比对及对其高分辨质谱数据的解析,鉴定为卡芬太尼。该方法可以用于实际案件的检测。A method was developed for the identification of carfentanil emerged in China by gas chromatography-mass spectrometry( GC-MS),ultra performance liquid chromatography-quadrupole time-of-flight-mass spectrometry( UPLC-Q-TOF MS) and Fourier transform infrared spectroscopy( FTIR). The power sample was extracted with methanol and water,and the supernatant was subjected and analyzed with GC-MS and UPLC-Q-TOF MS. For FTIR analysis,the power sample was placed in the attenuated total reflectance( ATR) accessory. One unknown component( tR= 13. 05 min) was detected by GC-MS,appearing its characteristic fragment ion peaks at m/z 303,105,243,187,96 and 154. It( tR= 3. 976 min) also was detected by UPLC-Q-TOF MS,with its characteristic fragment ion peaks [M + H]+( m/z 395. 2325) in the single stage and m/z 335. 2117,279. 1856,246. 1490,146. 0966,134. 0966,113. 0599 in the tandem( MS/MS) mode. FTIR-ATR spectra of the sample gave absorbance bonds at 1724,1635,1593,1352,1225 and 704 cm^-1. According to the information searched from NIST mass spectra library,the literatures and its high resolution mass spectrometry data,this target is identified as carfentanil. This method is suitable for the identification of carfentanil seized in an abuse new psychoactive substance market.
关 键 词:芬太尼类 卡芬太尼 气相色谱质谱联用(GC-MS) 超高效液相色谱-串联四极杆飞行时间质谱(UPLC-Q-TOF MS) 红外光谱(FTIR)
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