目的建立一种简便、快速、准确、可靠的GC-MS同时检测生物检材中的苯巴比妥、布洛芬、尼可刹米的方法.方法用p H=3-4的95%乙醇对生物检材进行浸泡,然后分别在p H=3-4及p H=10-11的条件下,用乙酸乙酯进行提取分离,GC-MS对样品进行分离分析,分别用总离子流图(TIC图)中苯巴比妥、布洛芬、尼可刹米的保留时间及质谱图中对应的特征离子碎片定性.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,苯巴比妥、布洛芬、尼可刹米定性的保留时间分别为8.472 min、7.087 min、6.655 min,苯巴比妥的特征离子碎片(m/z)为204及232;布洛芬的m/z为161及206;尼可刹米的m/z为106及177.结论该方法可用于法医毒物分析生物检材中苯巴比妥、布洛芬、尼可刹米的同时检测,结果令人满意.
Objective The study aimed to establish a kind of simple,rapid,accurate and reliable method in order to simultaneous determine the phenobarbital,ibuprofen and nikethamide in the biomaterial. Methods The biomaterial were pre-treated with ethanol(v/v 95%) at p H 3~4 and then was extracted with ethyl acetate at p H3~4 and 10~11, respectively. Finally, phenobarbital, ibuprofen and nikethamide in the biomaterial were simultaneous detected by GC-MS. The retention times and relevant characteristic fragment ions of the three substances in the total ion current(TIC) and the mass spectrogram could be used as the basis of qualitative analysis.Results The method was simple and easy operation. It has the characteristics of low background interference,good separation effect and fast analytical speed. The retention times of phenobarbital, ibuprofen and nikethamide were8.472 min, 7.087 min and 6.655 min,respectively. The characteristic fragment ions of phenobarbital were 204 and232(m/z), of ibuprofen were 161 and 206(m/z),and of nikethamide were 106 and 177(m/z). Conclusion The method showed a satisfactory result that it could be applied to simultaneous determine phenobarbital, ibuprofen and nikethamide of the biomaterial for forensic toxicological analysis.