A robust quantitative method was developed and validated for the analysis of eight volatile nitrosamines ((N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosodi-n-propylamine (NDPA), N-nitrosomorpholine (NMOR), N-nitrosopyrrolidine (NPYR), N-nitrosopiperidine (NPIP), and N-nitrosodi-n-butylamine (NDBA)) in a variety of tobacco matrices. Volatile nitrosamines are carcinogenic and are found in both tobacco and tobacco smoke. The method utilizes a Supported Liquid Extraction (SLE) sample preparation followed by gas chromatography (GC), and tandem mass spectrometry (MS/MS) with electron ionization (EI) for quantitation. Individually matched isotopically labeled internal standards were used for each analyte to ensure accurate quantitation through the sample preparation process. Validation was done for cigarette filler, smokeless tobacco, and roll-your-own tobacco matrices. Precision and accuracy values were assessed at three concentration levels and were excellent for all analytes. Accuracy values of 84 – 110% were observed for all analytes with an average recovery of 98.6%. Precision was &lt; 12% CV for all analytes with an average of 5.3%. Matrix effects were assessed using calibration curve slope comparison as well as spike accuracy to ensure accurate method application across all tobacco product types. The method detection limits ranged from 0.29 ng/g to 5.77 ng/g for the nitrosamines investigated. Accurate quantification of carcinogenic volatile nitrosamine quantitation will help in establishing the risks from tobacco use.

Volatile N-nitrosamines in tobacco matrices using isotope dilution gas chromatography-triple quadrupole tandem mass spectrometry

254th National Meeting (2017)

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