提出了气相色谱-串联质谱法测定血中巴比妥类药物(巴比妥、苯巴比妥、异戊巴比妥、司可巴比妥)含量的方法。样品以乙酸乙酯-环己烷(1+1)混合液为萃取剂,经快速溶剂萃取仪提取后,提取液用氮气吹干后以1.0 mL甲醇溶解,通过VF-5MS色谱柱分离,采用电子轰击离子源多反应监测模式进行质谱测定。4种巴比妥类药物的质量浓度与其峰面积均在10~1 000 μg·L-1之间呈线性关系,检出限(3S/N)在0.07~0.26 μg·L-1之间。以空白血液样品为基体进行回收试验,测得回收率在77.8%~93.4%之间,测定值的相对标准偏差(n=7)在2.3%~6.9%之间。

GC-MS/MS was applied to the determination of barbiturate drugs, i.e., barbital, amobarbital, secobarbital and phenobarbital, in blood. The sample was extracted with a mixture of ethyl acetate and cyclohenane (1+1) by accelerated solvent extraction, and the extract was evaporated to dryness by N2-blowing and dissolved with 1.0 mL of methanol. VF-5MS chromatrographic column was used for separation, and the multi-reactions monitoring with electron impact ionization source was adopted in MS. Linear relationships between values of peak area and mass concentration of the 4 barbiturate drugs were kept in the same range of 10-1 000 μg·L-1, with detection limits (3S/N) in the range of 0.07-0.26 μg·L-1. On the base of blank blood sample, test for recovery was made by standard addition method, values of recovery found were in the range of 77.8%-93.4%, with RSD′s (n=7) in the range of 2.3%-6.9%.