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目的为了应对毒鼠强急慢性中毒事件,建立高灵敏度与高准确度的气相色谱-质谱/质谱联用法(GC-MS/MS)测定毒鼠强的定性、定量方法。方法样品中的目标化合物用乙酸乙酯提取后,进行浓缩、定容,用GC-MS/MS进行测定。以毒鼠强的3个特征离子(m/z 131.9、m/z 211.9、m/z 239.9)作母离子,使用不同的电压进行碰撞,得到各自相应的子离子,选取分别来自3个母离子的共计5个离子对(239.9→41.9;239.9→132;211.9→131.9;211.9→92;131.9→42.1),以响应值较高的离子对(239.9→41.9)作为定量离子对,其余4个离子对作为定性离子对,采用多反应监测(MRM)方式进行测定。结果该方法在毒鼠强浓度范围为0.003μg/ml~2.0μg/ml时呈正相关,r=0.999 6,回收率为99.0%,RSD=5.1%,液体样品的检出限为0.000 03μg/ml(血液样品的检出限为0.000 2μg/ml),固体样品的检出限为0.000 1μg/g。结论所建立的GC-MS/MS测定毒鼠强的灵敏度高,选择性好,检出限低,适合毒鼠强痕量测定。
Objective To establish a qualitative and quantitative method for the determination of tetramine in rats by gas chromatography-mass spectrometry / mass spectrometry (GC-MS / MS) with high sensitivity and high accuracy in order to cope with acute poisoning and chronic poisoning. Method After the target compound in the sample was extracted with ethyl acetate, it was concentrated and its volume was determined by GC-MS / MS. The three characteristic ions of tetramine (m / z 131.9, m / z 211.9, m / z 239.9) were used as precursors and collided with different voltages to obtain their corresponding sub-ions. (239.9 → 41.9; 239.9 → 132; 211.9 → 131.9; 211.9 → 92; 131.9 → 42.1) with the highest response ion pair (239.9 → 41.9) as the quantitative ion pair. The other four ions As a qualitative ion pair, multiple reaction monitoring (MRM) was used. Results The method showed a positive correlation with strong concentration of tetramine in the range of 0.003μg / ml ~ 2.0μg / ml, r = 0.999 6, the recovery was 99.0%, RSD was 5.1%, and the detection limit was 0.000 03μg / ml (The detection limit of the blood sample is 0.000 2 μg / ml), and the detection limit of the solid sample is 0.000 1 μg / g. Conclusion The established tetracycline GC-MS / MS has strong sensitivity, good selectivity and low detection limit. It is suitable for the determination of tetramine in rats.