气相色谱-质谱法同时测定食物中毒样品中氟乙酰胺与毒鼠强

Simultaneous determination of fluoroacetamide and tetramine in the samples of food poisoning by gas chromatography-mass spectrometry

目的建立气相色谱-质谱法(GC-MS)同时测定食物中毒样品中氟乙酰胺与毒鼠强的方法。方法样品加入乙酰胺内标与适量氯化钠,用丙酮-乙酸乙酯(9∶1,V/V)混合溶液提取,采用GC-MS测定,氟乙酰胺采用内标法定量,毒鼠强用外标法定量。结果氟乙酰胺浓度在0.05μg/ml^10μg/ml时的相关系数为0.999 7,相对标准偏差为0.63%~1.52%(n=7),加标回收率为110%~122%(n=3),方法检出限为0.017 mg/kg;毒鼠强浓度在0.02μg/ml^10μg/ml时的相关系数为0.999 4,相对标准偏差为0.65%~3.02%(n=7),加标回收率为80.2%~104.0%(n=3),方法检出限为0.007 mg/kg。结论方法简便快速、准确度和灵敏度高,适用于食物中毒样品中氟乙酰胺与毒鼠强的测定。

Objective To develop a method for simultaneous determination of fluoroacetamide and tetramine in the samples of food poisoning by gas chromatography-mass spectrometry（ GC-MS）. Methods After adding the internal reference of acetamide and sodium chloride,fluoroacetamide and tetramine in the samples were extracted with acetone-ethyl acetate（ 9∶1,V / V）. The content of fluoroacetamide and tetramine in the extractions was measured by GC-MS. The internal standard method was used for quantitation of fluoroacetamide,while external standard method was used for tetramine. Results The correlation coefficient was 0. 999 7 under the fluoroacetamide concentration in the range of 0. 05 μg / ml-10 μg / ml. The relative standard deviations was in the range of 0. 63%-1. 52%（ n = 7）,and the rates of recovery ranged from 110%-122%（ n = 3）. The limit of detection of this method reached 0. 017 mg / kg. The correlation coefficient was 0. 999 4 under the tetramine concentration in the range of 0. 02 μg / ml-10 μg / ml. The relative standard deviations was in the range of 0. 65%-3. 02%（ n = 7）,and the rates of recovery ranged from 80. 2%-104. 0%（ n = 3）. The limit of detection of this method reached 0. 007 mg / kg. Conclusion This method is simple,fast,accuracy and sensitive so that it could be used for the determination of fluoroacetamide and tetramine in the samples of food poisoning.