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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

  • 摘要: 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5 μL。③确定的d-SPE净化剂为无水硫酸镁、N-丙基乙二胺(PSA)和C18粉末。④9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。

     

    Abstract: 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.

     

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