同位素稀释-气相色谱串联质谱法测定啤酒中4种亚硝胺类化合物

目的 建立啤酒中4种N-亚硝胺类化合物(N-亚硝基二甲胺、N-亚硝基二乙胺、N-亚硝基二丙胺、N-亚硝基二苯胺)的同位素稀释固相萃取-气相色谱串联质谱测定方法.方法 样品经活性炭固相萃取小柱富集、二氯甲烷洗脱,洗脱液经氮吹浓缩定容后,采用INNOWAX毛细管色谱柱分离,多反应监测(MRM)模式检测,同位素稀释内标法定量...

Determination of four N-nitrosamines in beer by isotope dilutiongas chromatography-tandem mass spectrometry

Abstract: Objective To establish an analytical method for determination of four N － nitrosamines ( N － nitrosodimethylamine, N － nitrosodiethylamine, N － nitrosodi － n － propylamine, N － nitroso diphenylamine) in beer samples by isotope dilution solid－ phase extraction and gas chromatography － tandem mass spectrometry( SPE － GC － MS /MS) . Methods N － nitrosamines in the samples were concentrated with activated carbon SPE column and eluted with dichloromethane. The eluent was concentrated to 1. 0 ml under nitrogen flow. The compounds were separated by INNOWAX capillary chromatographic column and detected in multiple reaction monitoring ( MRM) mode. Finally, the isotope dilution internal standard method was used for quantitative analysis. Results The substances had a good linear relationship in the range of 5 μg /L to 200 μg /L, with the correlation coefficients all greater than 0. 9995. The limits of detection ( LODs) were 0. 03 μg /L to 0. 10 μg /L and the limits of quantification ( LOQs) were 0. 10 μg /L to 0. 33 μg /L. The average recovery rates of different levels were 72. 1% － 100. 3% ,with the relative standard deviations ( RSDs) in the range of 1. 5% － 9. 5% . Conclusion The method is simple, sensitiveand accurate. And it is suitable for the detection of four N － nitrosamines in beer.