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研究了用基质固相分散-高效液相色谱质谱法测定吸烟者尿液中的烟草特有亚硝胺(TSNAs)。尿液样品浓缩后用碱性氧化铝分散处理,然后在带柱层析净化功能的索氏提取器中用氧化铝柱层析净化。经净化后样品中的TSNAs用UPLC-MS/MS分析。在选定条件下,四种烟草特有亚硝胺NAT、NNK、NNN和NAB的检出限分别为0.06,0.07,0.13,0.11 ng/m L,对样品进行7次测定,日内相对标准偏差为3.3%~4.9%;日间相对标准偏差为4.1%~4.9%,方法的回收率在82.3%~91.4%之间,结果令人满意。
The determination of tobacco-specific nitrosamines (TSNAs) in smokers urine by matrix solid phase dispersion-high performance liquid chromatography-mass spectrometry was studied. Urine samples were concentrated, dispersed in basic alumina and then purified by alumina column chromatography on a Soxhlet extractor with column chromatography purification. TSNAs in the purified samples were analyzed by UPLC-MS / MS. Under the selected conditions, the detection limits of the four tobacco-specific nitrosamines NAT, NNK, NNN and NAB were 0.06, 0.07, 0.13 and 0.11 ng / m L, respectively. The relative standard deviations 3.3% ~ 4.9%. The relative standard deviations during the day were 4.1% ~ 4.9%. The recoveries of the method ranged from 82.3% to 91.4%. The results were satisfactory.