【摘要】 提出了超高效液相色谱-串联质谱法测定烟草中N-亚硝基降烟碱(NNN)、N-亚硝基新烟草碱(NAT)、N-亚硝基假木贼碱(NAB)和4-甲基亚硝基吡啶基丁酮(NNK)等4种亚硝胺含量的方法。烟草样品经0.1mol.L-1乙酸铵溶液匀浆提取,离心分离取上清液过Waters AcquityUPLC BEH C18色谱柱(2.1mm×100mm,1.7μm)分离,以乙腈和0.01mol.L-1乙酸铵溶液按不同体积混合作流动相梯度洗脱。串联质谱测定中采用电喷雾离子源正离子模式和多反应监测模式检测,同位素内标法定量。NNK、NNN、NAB和NAT的检出限(3s)分别为0.06,0.17,0.15,0.053μg.L-1。方法的加标回收率在92.1%～104%之间;日内和日间相对标准偏差(n=7)分别为2.7%～3.3%和3.5%～4.2%。更多还原

【Abstract】 A method of UHPLC-MS/MS for the determination of 4 nitrosamines,including NNK,NNN,NAB and NAT,in tobacco was proposed.The sample was extracted with 0.1 mol·L-1 ammonium acetate solution by homogenization,after centrifugation,the supernatant was taken and separated on Waters Acquity UPLC BEH C18(2.1 mm×100 mm,1.7 μm) column,using the mixed solution of acetonifrile and 0.01 mol·L-1 ammonium acetate mixed in the different ratios as mobile phase for gradient elution.The contents of 4 nitrosamines were determined by MS/MS.The positive electrospray ionization and the multiple reactions monitoring mode were used in the detection.The isotope internal standard method was used to quantification for the 4 nitrosamines.Detection limit(3s) of NNK,NNN,NAB and NAT found were 0.06,0.17,0.15,0.053 μg·L-1 respectively.The proposed method was applied to the analysis of tobacco samples,giving values of recovery in the range of 92.1%-104%.Values of intra-day and inter-day RSD′s(n=7) were found in the ranges of 2.7%-3.3% and 3.5%-4.2% respectively.更多还原