啤酒和腊肠中N,N-二甲基亚硝胺的测定

Determination of N-dimethyl nitrosamine in beer and sausage

中文关键词:  N,N-二甲基亚硝胺  气相色谱-质谱法  内标法  啤酒  腊肠

英文关键词:N-dimethyl nitrosamine  gas chromatography-mass spectrometry  internal standard  beer  sausage

中文摘要:

      目的 建立气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)测定啤酒和腊肠中N,N-二甲基亚硝胺的方法。方法 试样经二氯甲烷超声提取、离心, SILICA/PSA玻璃柱净化后气相色谱/质谱仪直接测定, D6-N,N-二甲基亚硝胺内标法定量。结果 加标回收率范围为66.9%~103.4%, 相对标准偏差(RSD)在2.5%~7.7%。将该方法用于实际样品分析, 30份啤酒中均未检出N,N-二甲基亚硝胺, 8份腊肠样品中检出2份阳性样品, 含量均低于肉制品中N,N-二甲基亚硝胺限量值3.0 μg/kg。结论 此方法简便快速, 灵敏度较高, 可以用于啤酒和腊肠中N,N-二甲基亚硝胺的准确定量。

英文摘要:

      Objective To establish a method for the determination of N-dimethyl nitrosamine in beer and sausage by gas chromatography-mass spectrometry. Methods Homogenized samples sequentially were extracted by methylene chloride, centrifugation, and SILICA/PSA columns cleanup before analyzed by gas chromatography-mass spectrometry. Quantification of N-dimethyl nitrosamine was based on the use of D6-N-dimethyl nitrosamine. Results The present method showed acceptable recoveries of 66.9%~103.4%, with relative standard deviation (RSD) ranging from 2.5% to 7.7%. Analysis of 30 beer samples and 8 sausage samples by the current method were successfully performed. N,N-dimethyl nitrosamine were not detected in beer samples. Two positive sausage samples were detected and the content was lower than the limited value of 3.0 μg/kg in meat products. Conclusion This quantitative method is demonstrated to be rapid, simple, and high sensitive, which can be applied in the accurate determination of N-dimethyl nitrosamine in beer and sausage.