摘要
目的建立UPLC-MS/MS测定血痕中尼古丁、可替宁、甲基苯丙胺、氯胺酮、吗啡、O6-单乙酰吗啡、地西泮、三唑仑、艾司唑仑、佐匹克隆和利血平的方法。方法以甲醇为提取液,采用基质提取溶液配制标准溶液制作定量曲线。采用超高效液相色谱柱对待测样品进行分离;以电喷雾离子源正离子(ESI+)模式和多反应监测(MRM)模式进行质谱分析。优化实验条件,并进行方法学评价。结果选择UPLC HSS T3色谱柱,乙腈-5mmol/L甲酸铵+0.1%(v/v)甲酸作为流动相,甲醇作为提取溶剂。11种检测物检出限(S/N=3)和定量限(S/N=10)分别为0.04~2.82ng和0.13~7.64ng,1~500ng/mL范围内的线性关系良好。除利血平、吗啡外的检测物回收率为(53.8±5.3)%^(107.2±12.6)%。结论采用本文UPLC-MS/MS方法对血痕中11种常见烟草、毒品和药物成分进行检测,能够满足实际检案的要求,可在相关检验中选用。
Objective To develop an ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for nicotine, cotinine, methylamphetamine, cyclohexanone, morphine, O6- monoacetyl-morphine, diazepam, triazolam, estazolam, zopiclone and reserpine in blood spot. Methods The sample was extracted with methanol. The matrix-matched standard solutions were used to prepare the curve of quantitative analysis. The drugs were separated on an UPLC column. The mass spectrometric acquisition was carried out by means of electrospray ionization in positive mode （ ESI＋ ） with multiple reaction monitoring （MRM） method. Results The drugs were separated on a ACQUITY UPLC HSS T3 column while the mobile phase was fixed as acetonitrile ＋ 5mol/L HCOONH4 ＋ 0. 1% （v/v）HCOOH in water. Methanol was choosed as extraction solvent. The detection limits （ LOD, S/N = 3 ） and the quantification limits （ LOQ, S/N = 10） of the eleven drugs were 0. 04 -2.82ng and 0. 13 -7.64ng. The average recoveries ranged from（53.8 ±5.3）% to （ 107.2 ± 12.6） % except reserpine and morphine. Conclusion The UPLC-MS/MS method was adopted to analysis 11 common ingredients from tobacco, drug and medicine mixed in blood spot. It could be used in practice with fully satisfaction of analysis on crime scene.
出处
《中国法医学杂志》
CSCD
2014年第3期206-213,共8页
Chinese Journal of Forensic Medicine
基金
"十二五"国家科技支撑计划(2012BAK02B02)
公安部重点研究计划项目(2011ZDYJGAES002)
关键词
法医毒物分析
超高效液相色谱-串联质谱
血痕
代谢成分
forensic toxicological analysis
ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）
blood spot
metabolic components
