GC/MS法同时测定主流烟气中9种芳香胺

Simultaneous determination of nine aromatic amines in mainstream cigarette smoke by GC/MS

为检测卷烟主流烟气中的芳香胺,通过对样品前处理主要影响因素进行优化,建立了同时测定邻-甲苯胺(o-TOL)、间-甲苯胺(m-TOL)、对-甲苯胺(p-TOL)、2,6-二甲基苯胺(2,6-DMA)、邻-甲氧基苯胺(o-ASD)、1-萘胺(1-NA)、2-萘胺(2-NA)、3-氨基联苯(3-ABP)、4-氨基联苯(4-ABP)9种芳香胺的改进涡旋辅助分散液相微萃取(LPME)富集/分散固相萃取(d-SPE)净化-气相色谱质谱(GC/MS)分析方法。结果表明:(1)确定的涡旋辅助分散LPME富集条件为萃取溶剂甲苯,体积1.5 mL,盐析剂硫酸钠。(2)确定的衍生条件为衍生化试剂七氟丁酸酐,体积5μL。(3)确定的d-SPE净化剂为无水硫酸镁、N-丙基乙二胺(PSA)和C_(18)粉末。(4)9种芳香胺的检出限为0.03~0.08 ng/支,回收率为75.0%~127.3%,相对标准偏差(RSD)0.2%~9.6%。该方法前处理简便,适用于卷烟主流烟气中9种芳香胺的测定。

To determine nine aromatic amines in mainstream cigarette smoke, a modified vortex-assisted dispersive liquid phase microextraction （LPME） method coupled with gas chromatography-mass spectrometry （GC/MS） was developed by optimizing the main influencing factors of sample pretreatment. The analyzed nine aromatic amines were o-toluidine （o-TOL）, m-toluidine （m-TOL）, p-toluidine （p-TOL）, 2,6-dimethylaniline （2,6- DMA）, o-anisidine （o-ASD）, 1-naphthylamine （1-NA）, 2-naphthylamine （2-NA）, 3-aminobiphenyl （3-ABP） and 4-aminobiphenyl （4-ABP）. The results indicated that： 1） Using dispersive LPME, the best extraction solvent was toluene with the optimal volume of 1.5 mL, and Na2SO4 was chosen as the salting-out reagent. 2） For derivatization, heptafluorobutyric anhydride was selected as derivatization agent with the volume of 5 μL. 3） For d-SPE, the mixture of MgSO4, PSA and C18 was employed for cleanup. 4） The limits of detection for the nine aromatic amines ranged from 0.03 to 0.08 ng/cig. The recovery was from 75.0% to 127.3% with the relative standard deviations of 0.2%-9.6%. The developed method features simple sample pretreatment and is suitable for the determination of the nine aromatic amines in mainstream cigarette smoke.