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目的建立顶空-气相色谱质谱法测定血中正己烷代谢产物2,5-己二酮的方法。方法 3 ml血样加入内标物喹啉后,置70℃水浴40 min,经HP-5柱分离,内标工作曲线法定量。结果血中2,5-己二酮浓度在0.4μg/ml~1mg/ml时线性关系良好,相关系数为0.9994。方法的精密度相对标准偏差在5.7%~8.1%之间,血液样品加标回收率在89.2%~103.6%之间,方法检出限为0.2μg/ml。应用该法测定职业正己烷接触者53名和非正己烷接触者30名血中2,5-己二酮,结果显示职业正己烷接触者血中2,5-己二酮含量明显高于非正己烷接触者,并与接触正己烷浓度呈正线性相关(P<0.01)。结论建立的顶空气相色谱法测定2,5-己二酮方法简便、快速、干扰少,可用于职业接触正己烷的生物监测。
Objective To establish a method for the determination of 2,5-hexanedione in blood by headspace-gas chromatography-mass spectrometry. Method 3ml blood samples were added to the internal standard quinoline, set 70 ℃ water bath for 40 min, the HP-5 column separation, internal standard curve method. Results The concentration of 2,5-hexanedione in blood was good at 0.4μg / ml ~ 1mg / ml, the correlation coefficient was 0.9994. The relative standard deviations (RSDs) of the methods were between 5.7% and 8.1%. The spiked recoveries of blood samples ranged from 89.2% to 103.6%. The detection limit was 0.2μg / ml. This method was used to determine the presence of 2,5-hexanedione in blood of 53 n-hexane and non-n-hexane contact persons. The results showed that the content of 2,5-hexanedione in blood of occupational n-hexane was significantly higher than that of n-hexane Alkanes and showed a positive linear correlation with n-hexane concentration (P <0.01). Conclusion The established method for the determination of 2,5-hexanedione by headspace gas chromatography is simple, rapid, and less interference. It can be used for bio-monitoring of n-hexane in occupational exposure.