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

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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 establish a method for the simultaneous determination of fluoroacetamide and tetramine in food poisoning samples by gas chromatography-mass spectrometry (GC-MS). Methods The sample was added with acetamide internal standard and appropriate amount of sodium chloride and extracted with a mixed solution of acetone and ethyl acetate (9: 1, V / V). The content of fluoroacetamide was determined by GC-MS, Quantitative with external standard. Results The correlation coefficient of fluoroacetamide at the concentration of 0.05μg / ml ~ 10μg / ml was 0.999 7, the relative standard deviations were 0.63% ~ 1.52% (n = 7) and the recoveries were 110% ~ 122% 3). The detection limit of this method was 0.017 mg / kg. The correlation coefficient was 0.999 4 with the concentration of 0.02μg / ml ~ 10μg / ml. The relative standard deviation was 0.65% ~ 3.02% (n = 7) The standard recoveries ranged from 80.2% to 104.0% (n = 3). The limit of detection was 0.007 mg / kg. Conclusion The method is simple, rapid, accurate and sensitive. It is suitable for the determination of fluoroacetamide and tetramine in food poisoning samples.
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