提出了自动顶空-气相色谱-质谱联用检测血液中乙醇含量的方法.取一定量的血样或乙醇标准样品置于顶空瓶中(其中各加固定量的叔丁醇作为内标),在60 ℃及中速振摇的条件下平衡20 min,通过进样环定量地将一定量样品引入于气相色谱-质谱联用仪器中进行测定.乙醇和叔丁醇的保留时间分别为1.47 min和1.56 min.方法的线性范围为0.01~10.00 g·L-1,检出限(3S/N)为0.6 mg·L-1,测定下限(10S/N)为1.0 mg·L-1.乙醇的回收率在92%~105%之间,测定值的相对标准偏差(n=6)小于7%.

A method for the determination of ethanol in blood by GC-MS with auto-headspace sample introduction was proposed.The blood sample or ethanol standard (together with a definite amount of tert.-butanol as internal standard) was placed in the head-space bottle and equilibrated at 60 ℃ for 20 min with moderate-speed-shaking.Definite amount of sample was quantitatively introduced into the GC-MS instrument through the sample introduction loop.Retention time of ethanol and tert.-butanol was found at 1.47 min and 1.56 min,respectively.Linear relationship between values of peak area and mass concentration of ethanol was obtained in the range of 0.01-10.00 g·L-1 with values of detection limit (3S/N) of 0.6 mg·L-1 and lower limit of determination (10S/N) of 1.0 mg·L-1.The values of recovery of ethanol was found in the range from 92% to 105%,with RSD (n=6) less than 7%.