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法医学杂志 2017, Vol. 33 Issue (6) :619-621    DOI: 10.3969/j.issn.1004-5619.2017.06.011
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GC-MS法测定血中1-甲基海因含量及其法医学应用
高利娜,袁慧雅,徐恩宇,刘俊亭
(中国医科大学法医学院,辽宁 沈阳 110013)
Determination of 1-methylhydantoin Concentration in Blood by GC-MS Method and Its Application in Forensic Medicine
GAO LI-NA, YUAN HUI-YA, XU EN-YU, LIU JUN-TING
(School of Forensic Medicine, China Medical University, Shenyang 110013, China)

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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=0.015 51 x+0.007 26(R2=0.999 7),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。
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高利娜
袁慧雅
徐恩宇
关键词法医毒理学   气相色谱-质谱法   血液   1-甲基海因   代谢物     
Abstract: 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=0.015 51 x+0.007 26(R2=0.999 7) 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%, respectively. 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.
Keywordsforensic toxicology   gas chromatography-mass spectrometry   blood   1-methylhydantoin   metabolite     
Fund:

辽宁省教育厅科学研究一般项目(L2015570)

Corresponding Authors: 刘俊亭,男,教授,博士研究生导师,主要从事体内药毒物分析研究;E-mail:liujunting8@163.com   
About author: 高利娜(1983—),女,博士,副教授,主要从事体内药毒物分析研究;E-mail:gaolina0114@sina.com
引用本文:   
高利娜, 袁慧雅, 徐恩宇, 等.GC-MS法测定血中1-甲基海因含量及其法医学应用[J]  法医学杂志, 2017,33(6): 619-621
GAO LI-NA, YUAN HUI-YA, XU 恩YU, DENG , ET AL..Determination of 1-methylhydantoin Concentration in Blood by GC-MS Method and Its Application in Forensic Medicine[J]  , 2017,33(6): 619-621
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