GC-MS/MS测定毒鼠强中毒方法研究  

Study on detection method of tetramine intoxication by GC-MS/MS

作　　者：杜利敏[1] 袁野[1] 陈宁宁[1] 路守栋[1] 王龑[1] 

机构地区：[1]郑州市疾病预防控制中心,河南郑州450007

出　　处：《中国卫生检验杂志》2015年第5期629-632,共4页Chinese Journal of Health Laboratory Technology

摘　　要：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 In order to deal with the acute and chronic poisoning cases of tetramine,it is very necessary to establish a qualitative and quantitative method for detecting tetramine by Gas chromatography-mess spectrum（ GC-MS / MS） with high sensitivity and good accuracy. Methods The target compound of tetramine was concentrated after being extracted from samples with ethyl acetate,and then was analyzed by GC-MS / MS. Three characteristic ions of tetramine（ m / z 131. 9,m / z 211. 9,m / z 239. 9） as the parent ions were collided with different voltage,thereby their daughter ions could be acquired repectively.We selected an ion pair（ 239. 9 →41. 9） which has higher response value as quantitative iron pairs from 5 ion pairs（ 239. 9 →41. 9; 239. 9→132; 211. 9→131. 9; 211. 9→92; 131. 9→42. 1）,the other ion pairs as identification iron pairs. Detection was carried out by multiple reaction monitoring（ MRM）. Results The method showed a positive correlation in the concentration range of 0. 003 μg / ml ~ 2. 0 μg / ml of tetramine,r = 0. 999 6. The recovery rate was 99. 0%,and the relative standard derivations was 5. 1%. The detection limit of liquid sample was 0. 000 03 μg / ml（ 0. 000 2 μg / ml for blood sample）,and the detection limit of solid sample was 0. 000 1 μg / g. Conclusion This establishedmethod has a high sensitivity and accuracy,and it has a lower detection limit. It＇s suitable for the detection of trace amounts of tetramine.

关 键 词：毒鼠强 气相色谱-质谱/质谱 多反应监测 痕量 

分 类 号：O657.63[理学—分析化学]