An UPLC‐MS3 Method for Rapid Separation and Determination of Four Tobacco‐specific Nitrosamines in Mainstream Cigarette Smoke

Abstract

AbstractAn 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‐C18 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.