QuEChERS-气相色谱-串联质谱法测定熟肉制品中9种N-亚硝胺类化合物
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摘要
目的建立同时测定熟肉制品中9种N-亚硝胺类化合物的气相色谱-串联质谱分析方法。方法样品采用快速基质分散净化(QuEChERS)法处理后,用HP-INNOWax石英毛细管色谱柱(30 m×0.25 mm,0.25μm)分离,经气相色谱-串联质谱多反应监测技术进行定性及定量分析。结果 9种N-亚硝胺类化合物在0.20～50.00μg/kg范围内线性关系良好,相关系数均>0.997,方法检出限为0.02～0.1μg/kg。3个加标水平的平均回收率为78%～120%,相对标准偏差为3.42%～15.24%。结论本方法准确、快速、灵敏度高,可用于熟肉制品中9种N-亚硝胺类化合物的检测。
Objective A method was established for simultaneous determination of nine N-nitrosamines in cooked meat using enhance matrix removal QuEChERS-gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The samples were extracted by enhance matrix removal QuEChERS.The analytes were separated on a HP-INNOWax quartz capillary column(30 m×0.25 mm,0.25 μm), and ionized by electron impact ion source(EI).The data were collected by multiple reaction monitoring(MRM) mode,followed by qualitative screening and quantitative analysis. Results Nine N-nitrosamines had good linearities in the range of 0.20-50.00 μg/kg, with correlation coefficients above 0.997. The detection limits of were 0.02-0.1 μg/kg. The average recoveries of the nine N-nitrosamines were 78%-120% with relative standard deviations of 3.42%-15.24%.Conclusion The QuEChERS purification combined with GC-MS/MS method was rapid, accurate and sensitive,and suitable for the determination of nine N-nitrosamines in cooked meat.
Objective A method was established for simultaneous determination of nine N-nitrosamines in cooked meat using enhance matrix removal QuEChERS-gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The samples were extracted by enhance matrix removal QuEChERS.The analytes were separated on a HP-INNOWax quartz capillary column(30 m×0.25 mm,0.25 μm), and ionized by electron impact ion source(EI).The data were collected by multiple reaction monitoring(MRM) mode,followed by qualitative screening and quantitative analysis. Results Nine N-nitrosamines had good linearities in the range of 0.20-50.00 μg/kg, with correlation coefficients above 0.997. The detection limits of were 0.02-0.1 μg/kg. The average recoveries of the nine N-nitrosamines were 78%-120% with relative standard deviations of 3.42%-15.24%.Conclusion The QuEChERS purification combined with GC-MS/MS method was rapid, accurate and sensitive,and suitable for the determination of nine N-nitrosamines in cooked meat.
引文
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[10] 杨宁,陈颖慧,邓莉,等.双填料固相萃取-高效液相色谱/质谱法同时检测腌菜中9种N-亚硝胺[J].分析化学,2013,41 (7):1044-1049.
[11] 中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全国家标准食品中N-亚硝胺类化合物的测定:GB 5009.26—2016[S].北京:中国标准出版社,2016.
[12] 吴燕燕,刘法佳,李来好,等.GC-MS检测咸鱼中N-亚硝胺的条件优化[J].南方水产科学,2012,8(4):16-22.
[13] IRESUEUR C,KNITTL P,GARTNER M,et al.Analysis of 140 pesticides from convernational farming foodstuff samples after extraction with the modified QuEChERS method[J].Food Control,2008,19(9):906-914.
[14] 阮华,荣维广,宋宁慧,等.QuEChERS-在线凝胶色谱-气相色谱-质谱法测定植物油中34种农药残留[J].分析化学,2014,42(8):1110-1116.
[15] 赵博,邓美林,杨小珊,等.分散固相萃取-气相色谱串联质谱法测定动物源性食品中9种N-亚硝胺类化合物[J].色谱,2016,34(10):998-1004.
[2] 孙敬,郇延军,詹文圆,等.蒸煮火腿储藏期亚硝胺和亚硝酸钠含量的变化及其相关性研究[J].食品发酵工程,2008,34 (10):34-39.
[3] 中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全标准食品中污染物限量:GB 2762—2017[S].北京:中国标准出版社,2017.
[4] 李玲,徐幸莲,周光宏.气质联用检测传统中式香肠中的9种挥发性亚硝胺[J].食品科学,2013,34(14):241-244.
[5] 马强,席海为,王超,等.气相色谱-串联质谱法同时测定化妆品中的10种挥发性亚硝胺[J].分析化学,2011,39(8):1021-1027.
[6] 胡丽芳,尹德凤,周瑶敏,等.气质联用法测定咸鱼中N-二甲基亚硝胺含量[J].江西农业学报,2009,21(9):135-136.
[7] 赵华,王秀元,王萍亚,等.气相色谱质谱联用法测定腌制水产品中的挥发性N-亚硝胺类化合物[J].色谱,2013,31(3):223-227.
[8] 杨金川,杨莎莎,黄家岭.气相色谱-质谱法同时测定肉制品中9种N-亚硝胺的含量[J].贵州农业科学,2016,44 (11):155-158.
[9] 陈婷,温裕云,欧延,等.固相萃取净化及超高效液相色谱-串联质谱法测定橡胶制品中的13种N-亚硝胺[J].色谱,2014,32 (1):89-94.
[10] 杨宁,陈颖慧,邓莉,等.双填料固相萃取-高效液相色谱/质谱法同时检测腌菜中9种N-亚硝胺[J].分析化学,2013,41 (7):1044-1049.
[11] 中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全国家标准食品中N-亚硝胺类化合物的测定:GB 5009.26—2016[S].北京:中国标准出版社,2016.
[12] 吴燕燕,刘法佳,李来好,等.GC-MS检测咸鱼中N-亚硝胺的条件优化[J].南方水产科学,2012,8(4):16-22.
[13] IRESUEUR C,KNITTL P,GARTNER M,et al.Analysis of 140 pesticides from convernational farming foodstuff samples after extraction with the modified QuEChERS method[J].Food Control,2008,19(9):906-914.
[14] 阮华,荣维广,宋宁慧,等.QuEChERS-在线凝胶色谱-气相色谱-质谱法测定植物油中34种农药残留[J].分析化学,2014,42(8):1110-1116.
[15] 赵博,邓美林,杨小珊,等.分散固相萃取-气相色谱串联质谱法测定动物源性食品中9种N-亚硝胺类化合物[J].色谱,2016,34(10):998-1004.