GC-MS法测定血中1-甲基海因含量及其法医学应用

摘要

目的 建立全血中1-甲基海因的气相色谱-质谱(GC-MS)分析方法,为1-甲基海因相关法医学鉴定案件提供技术支持.方法 取0.5 mL血样,加入500 ng内标盐酸双苯戊二氨酯(SKF525A)、0.01 mol/L稀盐酸溶液2 mL,加入碳酸铵0.5 g调节pH值为9,加入乙酸乙酯2 mL,然后离心,取有机溶剂层,吹干后进行GC-MS分析.结果 血液中1-甲基海因在0.5～50 ng/mL范围内线性关系良好,线性回归方程为y=0.01551 x+0.00726(R2=0.9997),最低检出限为0.1 ng/mL,回收率为93.02％～108.12％,日内、日间精密度分别小于6.07％和13.37％.结论 本方法测定所得结果准确,重现性好,可用于血样中1-甲基海因含量的测定.%Objective To establish a gas chromatographic-mass spectrometric (GC-MS) analysis method for quantifying 1-methylhydantoin concentration in whole blood. To provide technical support to forensic identification related cases of 1-methylhydantoin. Methods As an internal standard, 500 ng SKF525A was added to 0.5 mL blood sample, and then 2 mL 0.01 mol/L dilute hydrochloric acid and 0.5 g ammonium carbonate were added in order to buffer the pH value to 9, and following 2 mL ethyl acetate. The organic solvent layer was obtained after centrifuge and then analysed by GC-MS after drying. Results Good linear relationship of 1-methylhydantoin in blood was obtained in the range of 0.5-50 ng/mL. The equation of linear regression was y=0.01551 x+0.00726(R2=0.9997) with 0.1 ng/mL detection limit, and the recovery was 93.02％-108.12％. The intra-day and inter-day precision were less than 6.07％ and 13.37％, respec-tively. Conclusion The results gotten by this method is accurate and reproducible, which can be used for the determination of 1-methylhydantoin concentration in blood samples.