吹扫捕集-气相色谱-质谱法测定啤酒中8种亚硝胺类化合物

Determination of 8 kinds of N-nitrosamine compounds in beer by purge-trap and gas chromatography-mass spectrometry

目的建立吹扫捕集-气相色谱-质谱法测定啤酒中8种亚硝胺类化合物的含量。方法啤酒通过吹扫捕集并经毛细管色谱柱分离,采用气相色谱-质谱法检测,以内标法定量。结果 8种亚硝胺类化合物（包括N-亚硝基二甲胺、N-亚硝基甲乙胺、N-亚硝基二乙胺、N-亚硝基二丙胺、N-亚硝基吡咯烷、N-亚硝基哌啶、N-亚硝基二丁胺和N-亚硝基二苯胺）在0.5~100.0μg/L的线性范围内呈现较好的线性关系,相关系数r均大于0.99。方法的检出限为0.20~0.35μg/L,平均回收率在78.1%~95.7%之间,相对标准偏差在2.5%~9.8%之间。结论该方法操作简单快捷,灵敏度和准确度均较高,可满足啤酒8种亚硝胺类化合物的检测。

Objective To establish a method for the determination of 8 kinds of N-nitrosamine compounds in beer by gas chromatography and mass spectrometry with purge-trap.Methods Beer samples were separated by capillary chromatographic column after purge-trap technique,and then determinated by gas chromatography and mass spectrometry.Internal standard method was used for quantitative analysis.Results Eight kinds of N-nitrosamine compounds（including N-nitrosodimethylamine（NDMA）,N-nitroso-Methyl ethylamine（NMEA）,N-Nitrosodiethylamine（NDEA）,N-nitrosodipropylamine（NDPA）,Nitrosopyrrolidine（NPYR）,Nitrosopiperidine（NPIP）,N-Nitrosodibutylamine（NDBA） and N-nitrosodiphenylamine（NPYL） had good linear relationships in the ranges of 0.5~100.0 μg/L,coefficients of 8 kinds of N-nitrosamine compounds were greater than 0.99.The limits of detection were between 0.2~0.35 μg/L,the average recoveries were in the range of 78,1%~95.7%,and the relative standard deviations were in the range of 2.5%~9.8%.Conclusion The method is simple,fast,sensitive and accurate,which can be used for the determination of 8 kinds of N-nitrosamine compounds in beer.