气相色谱-质谱法快速测定大米、面粉中氟乙酰胺和毒鼠强

Rapid determination of fluoroacetamide and tetramine in rice and flour by gas chromatography-mass spectrometer

目的建立大米、面粉中氟乙酰胺和毒鼠强的GC-MS法。方法样品采用乙酸乙酯提取,超声10 min,采用HP-INNOWAX色谱柱分离,选择离子检测(SIM)模式扫描,外标法定量。结果氟乙酰胺、毒鼠强线性相关系数均>0.99,方法定性限分别为0.015 mg/kg、0.013 mg/kg,定量限分别为0.044 mg/kg、0.040 mg/kg。在大米、面粉基质中3个添加水平的平均回收率为88.4%~93.7%,相对标准偏差(n=6)为3.8%~8.7%。结论该方法前处理简单快速、灵敏度高、峰形良好,准确度高,可对食物中毒大米及面粉样品中氟乙酰胺和毒鼠强进行准确快速的定性、定量分析。

Objective A gas chromatography-mass spectrometer(GC-MS)method was established for the determination of fluoroacetamide and tetramine in rice and flour.Methods The samples were extracted with ethyl acetate,sonicated for 10 minutes,separated by HP-INNOWAX chromatographic column,scanned by ion detection(SIM)mode,and quantified by external standard method.Results The linear correlation coefficients(r)of fluoroacetamide and tetramine were greater than 0.99.The qualitative limits of the method were 0.015 and 0.013 mg/kg,respectively,and the quantitative limits were 0.044 mg/kg and 0.040 mg/kg,respectively.The average recovery of the three levels of addition in rice and flour matrix was 88.4%-93.7%,and the relative standard deviation(n=6)was 3.8%-8.7%.Conclusion This method is simple and rapid,with high sensitivity,good peak shape and high accuracy.It can be used for accurate and rapid qualitative and quantitative analysis of fluoroacetamide and tetramine in rice and flour samples in food poisoning.