摘要
提出了气相色谱-串联质谱法测定无烟气烟草中N,N-二甲基亚硝胺的方法。无烟气烟草样品(0.500g)用二氯甲烷10mL超声萃取,上清液用硅固相萃取柱净化。在气相色谱分离中用DB-WAX石英毛细管色谱柱为固定相,在质谱分析中采用多反应监测模式。采用内标法定量。N,N-二甲基亚硝胺的线性范围为0.2~10μg·L^(-1),方法的检出限(3s)为0.018ng·g^(-1),测定下限(10s)为0.060ng·g^(-1)。在3,6,10ng等3个浓度水平进行加标回收试验,回收率为94.7%~101%,测定值的相对标准偏差(n=5)为2.8%~6.8%。
A method of GC-MS/MS for the determination of N-nitrosodimethylamine in smokeless tobacco was proposed.The sample of smokeless tobacco（0.500 g） was extracted ultrasonically with 10 mL of dichloromethane and the supernatant was purified with Si solid phase extraction column.The DB-WAX quartz capillary chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS determination.Internal standard method was used for quantitative.Linearity range of Nnitrosodimethylamine was found between 0.2μg·L^（-1） and 10μg·L^（-1） with detection limit（3s）of 0.018ng·g^（-1）and lower limit of determination（10s）of 0.060ng·g^（-1）.Tests for recovery were made by standard addition method at the concentration levels of 3,6,10 ng,giving values of recovery and RSD′s（n=5）in the ranges of 94.7%-101% and 2.8%-6.8% respectively.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第8期917-922,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
