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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 establish a UPLC-MS / MS method for the determination of nicotine, cotinine, methamphetamine, ketamine, morphine, O6-monoacetylmorphine, diazepam, triazolam, estazolam, zopiclone and reserpine Methods. Methods Methanol was used as the extract, and the matrix extract solution was used to prepare the standard solution to make the quantitative curve. The samples were separated by Ultra Performance Liquid Chromatography (HPLC) and analyzed by electrospray ionization positive ion (ESI +) mode and multiple reaction monitoring (MRM) mode. Optimization of experimental conditions, and methodological evaluation. Results The UPLC HSS T3 column was used. The mobile phase consisted of acetonitrile - 5mmol / L ammonium formate + 0.1% (v / v) formic acid and methanol as the extraction solvent. The detection limits (S / N = 3) and the limit of quantification (S / N = 10) of 11 samples were 0.04-2.82ng and 0.13-7.64ng, respectively. The linearity was good in the range of 1-500ng / mL. In addition to reserpine, the detection rate of morphine outside the recovery was (53.8 ± 5.3)% ~ (107.2 ± 12.6)%. Conclusion The UPLC-MS / MS method is used to detect 11 kinds of common tobacco, drugs and drug components in bloodstains, which can meet the requirements of actual inspection and can be used in relevant tests.