Quantitative Estimation of Some Volatile N-Nitrosamines in Tobacco Smoke Using Validated GC-MS Method
More details
Hide details
Petre Melikishvili Physical and Organic Chemistry, Ivane Javakhishvili Tbilisi State University, 0186, Anna Politkovskaya Str., Tbilisi, Georgia
Imeda Rubashvili   

Petre Melikishvili Physical and Organic Chemistry, Ivane Javakhishvili Tbilisi State University, 0186, Anna Politkovskaya Str., Tbilisi, Georgia
Publication date: 2017-10-05
Eurasian J Anal Chem 2014;9(2):79–91
The aim of this work was the quantitative estimation of some volatile N-nitrosamines in tobacco smoke of local cigarette different brands using an efficient, rapid and sensitive GC-MS method which was validated before. The chromatographic system suitability was tested by using the following characteristics: The RSD, % of peak areas (five replicate injections) was <2.0 %; The RSD, % of retention times <1.0 %; the number of theoretical plates was > 2000; the tailing factor < 2.0; the resolution between the two nearest peaks >2.0 for all N-nitrosamines. The calibration curve was linear over a concentration range 0.5 - 100 µg mL-1 with a correlation coefficient >0.99. The LOD and LOQ were 0.25 µg mL-1 and 0.5 µg mL-1, respectively. This method can be used to determine nine volatile N-nitrosamines namely N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosodipropylamine (NDPA), N-nitrosodibutylamine (NDBA), N-nitrosopiperidine (NPIP), N-nitrosopyrrolidine (NPYR), N-nitrosomorpholine (NMPA), N-nitrosodiphenylamine (NDPA) diluted in solvent - methanol as a sample solution which can be obtained from tobacco smoke or solid/liquid material using extraction. The determined quantities of some volatile N-nitrosamines - NDMA, NMEA and NDEA in tobacco smoke vary 190 - 320, 87 – 119 and 99 – 166 ng/cigarette, respectively.
Hiramoto K, Ohkawa T and Kikugawa K (2001) Release of nitric oxide together with carbon-centered radicals from N-nitrosamines by ultraviolet light irradiation. Free Rad. Res. 35:803–813.
Scanlan AR (2000) Nitrosamines and Cancer, The Linus Pauling institute. Available at http://lpi.oregonstate.edu/f-w.... Last updated November, 2011.
Mangino MM and Scanlan AR (1981) N-nitrosamines in beer, N-Nitroso Compounds. ACS Symposium Series 174:229–245.
Neurath G, Pirmann B, Lüttich W and Wichern H (1964) N-nitroso compounds in tobacco smoke. Contributions to Tobacco Research 3:251-262.
Qian M, Wei XH, Chao W, Hua B, Cheng XG, Ning S, Yan XL and Bing WJ (2011) Determination of ten volatile nitrosamines in cosmetics by gas chromatography tandem mass spectrometry. Chinese Journal of Analytical Chemistry 39:1201-1207.
Walters CL, Johnson EM and Ray N (1970) Separation and detection of volatile and non-volatile N-nitrosamines. Analyst 95:585-589.
Matyska MT, Pesek JJ and Yang L (2000) Screening method for determining the presence of N-nitrosodiethanolamine in cosmetics by open-tubular capillary electrochromatography. J. Chromatogr. A 887:487-503.
Filho PJS, Valcarcel M, Rios A, Zanin KD and Caramoa EB (2003) Determination of nitrosamines in preserved sausages by solid-phase extraction-micellar electro-kinetic chromatography. J. Chromatogr. A 985:503-512.
Bellec GF, Cauvin MC, Calve KL, Dreano Y, Gouerou H, Menez JF and Berthou F (1996) Analysis of N-nitrosamines by high-performance liquid chromatography with post-column photohydrolysis and colorimetric detection. J. Chromatogr. A 727:83-92.
Chen A, Huebschmann HJ, Fangyan L, Foong CY and Harn CS, High Sensitivity Analysis of Nitrosamines Using GC-MS/MS (2012) Alpha Analytical Pte. Ltd., Thermo Fisher Scientific, Health Sciences Authority, HAS Singapore.
Brunnemann DK and Hoffmann D (1991) Analytical studies on tobacco-specific Nnitrosamines in tobacco and tobacco smoke. Crit. Rev. Toxicol. 21:235-240.
Sannino A and Bolzoni L (2013) GC/CI-MS/MS method for the identification and quantification of volatile N-nitrosamines in meat products. Food Chem. 141(4): 3925- 3930.
Seyler TH, Kim JG, Hodgson JA, Cowan EA, Blount BC and Wang L. (2013 )Quantitation of urinary volatile nitrosamines from exposure to tobacco smoke. J Anal Toxicol. 37(4):195-202.
Zhao H, Wang X, Wang P, Zhou Y, Xue C, Jiang L (2013) Determination of volatile N-nitrosamine compounds in salted aquatic products by gas chromatography-mass spectrometry. Chinese Journal of Chromatography 31(3):223-227.
Munch JW and Bassett MV. EPA Document #:EPA/600/R-05/054: Method 521: Determination of nitrosamines in drinking water by solid phase extraction and capillary column gas chromatography with large volume injection and chemical ionization tandem mass spectrometry (MS/MS) (Version 1.0) U.S. Environmental Protection Agency (2012).
International Organization for Standardization (ISO): International Standard ISO 5725-2: Accuracy of Measurement Methods and Results – Part 1: General Principles and Definitions, ISO, Geneva, Switzerland (1994).
Guide to the Evaluation of Measurement Uncertainty for Quantitative Test Results, European Federation of National Associations of Measurement, Testing and Analytical Laboratories, Technical Report No. 1/2006, EUROLAB Technical Secretariat, Paris (2006).
Assessment of Uncertainties of Measurement for Calibration and Testing Laboratories, Second Edition. c RR Cook, Published by National Association of Testing Authorities, Australia (2002).
Guide for evaluation of uncertainty in calibration, International accreditation service, INC, CA 90601 USA, (2008).
ICH Harmonized tripartite guideline: Validation of analytical procedures: text and methodology, Q2 (R1) (2005).
Ermer J and Miller JH (2005) Method Validation in Pharmaceutical Analysis, WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim, p. 403.
Eurachem Guide: The Fitness for Purpose of Analytical Methods – A Laboratory Guide to Method Validation and Related Topics, 2nd ed. (2014).