啤酒中N-亚硝胺的SPME-GC-MS分析

Determination of Volatile N-nitrosocompounds in Beer by SPME-GC-MS

研究了固相微萃取-气相色谱-质谱(SPME-GC-MS)联用方法检测啤酒中的N-亚硝基二乙胺(NDEA)、N-亚硝基吡咯烷(NPYR)、N-亚硝基二丁胺(NDBA),采用聚二甲基硅氧烷／二乙烯苯(PDMS／DVB)萃取头,对影响固相微萃取效率的萃取时间、搅拌速度以及萃取方式等进行了优化,在优化实验条件下,方法的线性范围在12.5～250μg／L之间,相关系数r为0.9971～0.9995,检出限分别为NDEA4.50μg／L,NPYR8.99μg／L,NDBA2.27μg／L,NDBA回收率为86%～96%,相对标准偏差6.2%～8.9%,该法简化了前处理步骤,快速、方便,结果满意。

A solid-phase microextraction(SPME)coupled with gas chromatography-mass spectrometry has been used for determination of N_nitrosodiethylamine,N_nitrosodi_ n_butylamine,N_nitrosopropylamine in beer.A polydimethylsiloxane/divinylbenzene coated fiber was used.The experimental conditions,such as extraction time,stirring speed and the way of extraction,were optimized.The linear range was between12.5and250μg/L with the detection limits of2.27to8.99μg/L.The average recoveries of NDBA were86%～96%and the RSD was6.2%～8.9%.It is a solvent_saving,environmentally beneficial new method with satisfactory results.