UPLC-MS/MS和主成分分析法判别海洛因原产地  

Classification of heroin by UPLC-MS/MS and principal component analysis

作　　者：刘翠梅[1,2] 花镇东[2] 白燕平[2] 

机构地区：[1]中国人民公安大学刑事科学技术系,北京100038 [2]公安部禁毒情报技术中心,北京100193

出　　处：《分析试验室》2013年第8期35-39,共5页Chinese Journal of Analysis Laboratory

基　　金：国家科技支撑计划(No.2011BAK04B06)资助

摘　　要：建立了超高效液相色谱-串联四极杆质谱仪(UPLC-MS-MS)在电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式下定量测定海洛因中9种生物碱的方法,并采用主成分分析法建立数学模型,实现了快速区分"东南亚"和"西南亚"地区海洛因样品的目的。样品使用甲醇超声提取,ACQUITY UPLC BEH C18(100 mm×2.1 mm i.d.,1.7μm)色谱柱,流动相为pH 9.66的10 mmol/L的碳酸氢铵和乙腈,在梯度条件下分析。结果表明,在5～500μg/kg添加水平下回收率范围为88%～118%,相对标准偏差为1.7%～10%。9种生物碱的检出限(LOD,以信噪比(S/N)>3计)和定量限(LOQ,以S/N>10计)分别为0.03～1.67 mg/kg和0.10～5.51 mg/kg。本方法在11 min内即可对缴获海洛因样品中的9种生物碱进行定量分析,可用于海洛因原产地的快速判别。A novel method has been developed for the determination of 9 alkaloids in heroin samples by ultra performance liquid chromatography combined with tandem mass spectrometry（UPLC-MS-MS）.For MS/MS detection,an atmospheric pressure positive electrospray source was employed with multiple reaction monitoring（MRM）.A mathematical model was also developed on the basis of principal components analysis（PCA）,which can be used to classify the heroin sample from ＂SEA＂and ＂SWA ＂.The sample was extracted by ultrasonic,using methanol as a solvent.An ACQUITY UPLC BEH C18 column（100 mm × 2.1 mm i.d.,1.7 μm） with binary gradients containing 10 mmol/L ammonium bicarbonate（pH 9.66） /acetonitrile mixtures was investigated for the analysis.The average recoveries at 5 ～ 500 μg/kg ranged from 88% to 118% and RSD were 1.7% ～ 10.3%.The detection limits（LOD,S/N 3） and the quantification limits（LOQ,S/N 10） of the 9 alkaloids were 0.03 ～ 1.67 mg/kg and 0.10 ～ 5.51 mg/kg,respectively.The method is rapid,simple,accurate and highly sensitive.The quantitative analysis of 9 alkaloids in heroin samples could be finished within 11 minutes,which is conducive to the rapid determination of heroin geographical source.

关 键 词：海洛因 超高效液相色谱-串联四极杆质谱 生物碱 原产地 

分 类 号：O657.7[理学—分析化学]