Objective To establish a kind of simple ,rapid ,accurate and reliable method to determine the phenobarbital in the biomaterial .Methods We pre‐treated biomaterial by the method that the reagent of acetone∶water (v/v 8∶2) was firstly used to soak the biomaterial ,and then we took use of ethyl acetate as reagent to extract the phenobarbital of the biomaterial in the present of pH=3-4 .We finally employed GC‐MS to determine these samples .On the one hand ,we not only took advantage of the reten‐tion time of the phenobarbital in total ion current (TIC) but also took advantage of the characteristic fragment ions of phenobarbital in mass spectrogram as qualitative basis .On the other hand ,we took advantage of the external standard method as quantitative ba‐sis .Results The method had the characteristics of the simple and easy operation .There was hardly background interference and there was good separation effect in the method .The method also had the characteristics of fast analytical speed such as the retention time of the phenobarbital was 8 .385 min .The characteristic fragment ions of phenobarbital was m/z 204 and m/z 232 .The charac‐teristic fragment ions of m/z 204 was served as quantitative ion fragments and we employed the external standard method to quanti‐fy in the method .In short ,the average recovery rate of the method was 87 .35% .Relative standard deviation (RSD) was 5 .43% in the method .The lowest limit of detection (LLOD) was 0 .005 mg/mL .Conclusion The method showes satisfactory result that it could be applied to determine the phenobarbital of the biomaterial of forensic toxicological analysis .%目的：建立一种简便、快速、准确、可靠的方法检测生物检材中的苯巴比妥。方法丙酮∶水（8∶2）对生物检材进行浸泡，然后在pH值为3～4条件下，采用乙酸乙酯进行提取分离，气相‐质谱联用（GC‐MS）对样品进行检测，使用总离子流图（TIC图）中苯巴比妥保留时间及质谱图中苯巴比妥的特征离子碎片定性，应用外标法进行定量。结果该方法简单易操作，背景干扰小，分离效果好，分析速度快，用于苯巴比妥定性的保留时间为8．385 min ，苯巴比妥的特征离子碎片为m／z 204和m／z 232；以m／z 204为定量离子碎片，采用外标法进行定量，回收率为87．35％，相对标准偏差RSD为5．43％，最低检出限（LLOD）为0．005 mg／mL。结论该方法可用于法医毒物分析生物检材中苯巴比妥的检验，效果良好。
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