基质固相分散-UPLC-MS／MS 法测定吸烟者尿液中的 TSNAs

摘要

A matrix solid phase dispersion and ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) method for the determination of tobacco specific N-nitrosamines (TSNAs) in the urine sample of smoker was studied .The concentrated urine samples were dispersed with silica gel . Then the samples were purified by alkaline aluminum oxide column chromatography combined with cable extraction.The TSNAs in purified samples were analyzed by ultra performance liquid chromatography tan-dem mass spectrometry.The limits of detection for NAT,NNK,NNN and NAB were 0.06,0.07,0.13, 0.11 ng/mL.The repeatability of method ranged from 3.3% to 4.9% and the recoveries were from 82.3%to 91.4%.This method was applied to the determination of TSNAs in the urine samples of smoker with good results .%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／mL，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。