摘要

An ultra-high-pressure liquid chromatography/MS3 (UPLC-MS3) method has been developed and validated for the quantitative determination of four major TSNAs in mainstream cigarette smoke using MS3 scan mode on a hybrid triple quadrupole-linear ion trap mass spectrometer. The new method combining the UPLC with MS3 scan mode offers decreased sample analysis time and good selectivity. After mainstream cigarette smoke was collected on a Cambridge filter pad, the particulate matter was extracted with ammonium acetate solution and analyzed by UPLC-MS3 using isotopically labeled analogues as internal standards. Four TSNAs were completely separated on an Agilent XDB-C-18 UPLC column using isocratic elution during a 6 min LC run time. Excellent linearity was obtained over the concentration range of 1.0-150.0 ng/mL for all TSNAs with values for correlation coefficient (r) between 0.9985-0.9994. Limits of detection (LOD) of each TSNA varied from 0.023 to 0.067 ng/mL, and lower limits of quantification (LLOQ) varied from 0.077 to 0.223 ng/mL, respctively. The recovery of each TSNA was from 89.2 to 106.8%. The method achieved excellent reproducibility with RSD 2.1-6.8% for intra-assay and 3.4-9.1% for inter-assay. This method can be used as an effective approach to significantly improve the detection capability for TSNAs in complex matrices.