气相色谱-质谱法测定肉制品中的9种挥发性N-亚硝胺类物质

摘要

This research has established a rapid detection method for nine volatile N-nitrosamines in meat and meat products by using gas chromatograph-mass spectrometry (GC-MS). In this experiment, we investigated the effect of extraction solvent type and chromatographic conditions on the extraction and separation of the target compounds. Meanwhile, comparison of solid-phase extraction (SPE) cartridges packed with acidic alumina, C18, activated carbon or PSA, or both C18 and PSA was carried out for the purification of the N-nitrosamines. Results showed that the linear range of the proposed method was 0‒10 μg/mL with correlation coefficients more than 0.999 2. Good reproducibility was observed with relative standard deviation (RSD) not exceeding 3.2% and the mean recoveries were in the range of 85%‒98%. The detection limits for N-nitrosodimethyl amine (NDMA), N-nitrosomethyl ethyl amine (NMEA), N-nitro sodibutyl amine (NDBA) and six other N-nitrosamines were 1.0, 2.1, 0.8 and 0.5 mg/kg, respectively. This method can meet the requirement for the determination of N-nitrosamine residues in meat and meat products.%研究建立一种适用于肉制品中9种挥发性N-亚硝胺含量的气质联用快速检测方法。实验优化提取溶剂和色谱柱对提取和分离检测影响的条件，同时考察4种固相萃取单柱（酸性氧化铝、C18、活性炭、PSA）和1种双填料的混合固相萃取柱（PSA-C18）的净化效果。结果表明：本检测方法的线性系数均可达到0.9992以上；线性范围为0～10μg/mL；重现性良好，相对标准方差均≤3.2%；回收率为85%～98%；检测限分别为N-亚硝基二甲基胺1.0μg/kg、N-亚硝基甲基乙基胺2.1μg/kg、N-亚硝基二丁基胺0.8μg/kg；其他均为0.5μg/kg。该方法能够满足测定肉及肉制品中N-亚硝胺的残留含量的需要。