气相色谱-飞行时间质谱测定毒鼠强精确质量及其在生物样品检测中的应用

Determination of Exact Mass of Tetramine by Gas Chromatography-Time-of-Flight Mass Spectrometry and Its Application in Biosamples

应用气相色谱-飞行时间质谱(GC-TOFMS)和自建质量校正方法测定了剧毒鼠药-毒鼠强精确离子质量,质量误差小于2 m amu(毫原子质量单位),推测出离子元素组成为C4H8N4O4S2,提高了定性分析的准确性;用选择质量色谱和内标法,毒鼠强在0.10～10.0 mg/L成线性,相关系数大于0.999,仪器检出限为40pg(信噪比>5);用液-液萃取GC-TOFMS测定了某城市特大毒鼠强中毒事件的有毒食品和中毒者样品,均检出毒鼠强;并利用检测结果可对治疗效果予以评估。

The exact mass of poisonous rodenticide tetramine (C4H8N4O4S2, accurate mass 239. 9987) was determined by gas chromatography-time of flight mass spectrometry (GC-TOFMS) with home-made mass calibration method. The elemental composition of the molecular ion was determined to be C4H8N4O4S2 with mass error less than 2 mamu. The calibration curve of tetramine is linear (correlation coefficient: 0. 999) within the range of 0. 10 -10. 0 mg/L using n-C15H32 as internal standard. The limit of detection is 40 pg(S/N>5). The samples of a city in southern China were analyzed by liquid-liquid extraction and GC-TOFMS, and tetramine was detected in food and serum samples taken from site and poisoned victims. The results are used to evaluate the therapic effect of the poisoned persons.