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目的建立复杂食品和呕吐物中氟乙酰胺和毒鼠强的气相色谱-质谱(GC-MS)法。方法先用乙酸乙酯提取食品及呕吐物中的氟乙酰胺、毒鼠强,然后采用乙腈、正己烷液液分配,SILICA/PSA固相萃取柱净化、洗脱液浓缩后,用气相色谱-质谱仪测定。结果当浓度为0.1μg/ml~20.0μg/ml时,测定的氟乙酰胺和毒鼠强均呈良好的线性关系,r≥0.999 0。样品加标量为0.10 mg/kg、0.20 mg/kg、1.00 mg/kg时,回收率为71.4%~92.6%,RSD为1.7%~5.7%。氟乙酰胺的检出限为0.01 mg/kg,毒鼠强的检出限为0.02 mg/kg。结论本方法能有效去除样品中的杂质对氟乙酰胺和毒鼠强测定的干扰,方法准确可靠,灵敏度高,适用于呕吐物及复杂食品中氟乙酰胺和毒鼠强的同时检测。
Objective To establish a gas chromatography-mass spectrometry (GC-MS) method for the determination of fluoroacetamide and tetramine in complex food and vomit. Methods Fluoroacetamide and tetramine in food and vomit were extracted firstly with ethyl acetate, and then liquid-partitioned with acetonitrile and n-hexane, cleaned up with SILICA / PSA solid-phase extraction column, and the eluate was concentrated and identified by gas chromatography- Mass spectrometry. Results When the concentration was 0.1μg / ml ~ 20.0μg / ml, the determination of fluoroacetamide and tetramine strong showed a good linear relationship, r ≥ 0.9999. The recoveries ranged from 71.4% to 92.6% and the RSDs ranged from 1.7% to 5.7% with the addition of 0.10 mg / kg, 0.20 mg / kg and 1.00 mg / kg respectively. The detection limit of fluoroacetamide was 0.01 mg / kg, and the detection limit of tetramine was 0.02 mg / kg. Conclusion This method can effectively remove the interference of the impurities in the sample on the determination of fluoroacetamide and tetramine. The method is accurate and reliable and has high sensitivity. It is suitable for the simultaneous detection of fluoroacetamide and tetramine in vomit and complex foods.