Determination of NOx in Mainstream Cigarette Smoke, CORESTA Collaborative Study and Recommended Method

Tayyarah, Rana; Sirkisoon, Leona R.; Morton, Michael J.; Walker, Aidan M.; Schmidt, Thomas

doi:10.2478/cttr-2025-0020

Abstract

A collaborative study among twelve laboratories was conducted to establish a recommended method for determination of oxides of nitrogen (NOx) in mainstream cigarette smoke. Three cigarette samples, with ISO 3308 total particulate matter yields ranging from 2–17 mg/cig, were evaluated under both a non-intense (ISO 3308) and an intense (ISO 20778) smoking regime to assess the method’s applicability across a range of conditions. Mainstream cigarette smoke was either passed through an in-line detector or collected in a gas-tight system for offline determination of NO_x by chemiluminescence. Optional use of glass fiber filter pads enabled gravimetric determination of total particulate matter. Statistical analyses were performed according to ISO 5725 to determine repeatability (r) and reproducibility (R), and z-scores. Reproducibility, expressed as a percentage of mean yield across all products, smoking regimes, and analysis types, ranged from 15.1–49.7%. NO_x yields ranged from 71–437 μg/cig and followed expected trends with respect to total particulate matter and smoking intensity. These results demonstrate the robustness of the proposed method and support its adoption as CORESTA Recommended Method CRM N° 104. [Contrib. Tob. Nicotine Res. 34 (2025) 222–229]

References

El-Mahdy, M.A., T.M. Abdelghany, C. Hemann, M.G. Ewees, E.M. Mahgoup, M.S. Eid, M.T. Shalaan, Y.A. Alzarie, and J.L. Zweier: Chronic Cigarette Smoke Exposure Triggers a Vicious Cycle of Leukocyte and Endothelial-Mediated Oxidant Stress that Results in Vascular Dysfunction; Am. J. Physiol. Heart Circ. Physiol. 319 (2020) H51–H65. DOI: 10.1152/ajpheart.00657.2019
Open DOI Search in Google Scholar Back to article
Vleeming, W., B. Rambali, and A. Opperhuizen: The Role of Nitric Oxide in Cigarette Smoking and Nicotine Addiction; Nicotine Tob. Res. 4 (2002) 341–348. DOI: 10.1080/14622200210142724
Open DOI Search in Google Scholar Back to article
Church, D.F. and W.A. Pryor: Free-Radical Chemistry of Cigarette Smoke and its Toxicological Implications; Environ. Health Perspect. 64 (1985) 111–126. DOI: 10.1289/ehp.8564111
Open DOI Search in Google Scholar Back to article
Philippe, R.J. and E. Hackney: The Presence of Nitrous Oxide and Methyl Nitrite in Cigarette Smoke and Tobacco Pyrolysis Gases; Tob. Sci. 3 (1959) 139–143.
Search in Google Scholar Back to article
Bokhoven, C. and H. Niessen: Amounts of Oxides of Nitrogen and Carbon Monoxide in Cigarette Smoke, with and without Inhalation; Nature 192 (1961) 458–459. DOI: 10.1038/192458a0
Open DOI Search in Google Scholar Back to article
Norman, V. and C. Keith: Nitrogen Oxides in Tobacco Smoke; Nature 205 (1965) 915–916. DOI: 10.1038/205915b0
Open DOI Search in Google Scholar Back to article
Klimisch, H.J. and E. Kirchheim: Quantitative Determination of Nitrogen Oxide in Cigarette Smoke by Means of Chemiluminescence; Z. Lebensm. Unters. Forsch. 163 (1977) 48–52. DOI: 10.1007/BF01123557
Open DOI Search in Google Scholar Back to article
Jenkins, R.A. and B.E. Gill: Determination of Oxides of Nitrogen (NO_x) in Cigarette Smoke by Chemiluminescent Analysis; Anal. Chem. 52 (1980) 925–928. DOI: 10.1021/ac50056a035
Open DOI Search in Google Scholar Back to article
Cueto, R. and W.A. Pryor: Cigarette Smoke Chemistry: Conversion of Nitric Oxide to Nitrogen Dioxide and Reactions of Nitrogen Oxides with Other Smoke Components as Studied by Fourier Transform Infrared Spectroscopy; Vibr. Spectros. 7 (1994) 97–111. DOI: 10.1016/0924-2031(94)85045-3
Open DOI Search in Google Scholar Back to article
Health Canada: Health Canada Official Method T-110 – Determination of Oxides of Nitrogen in Mainstream Tobacco Smoke. Available at: https://health.canada.ca/apps/open-information/tobacco/100PDF/T-110E.PDF (accessed November 2025)
Search in Google Scholar Back to article
Wu, D., W. Gu, W. Xie: Determination of Oxides of Nitrogen in Mainstream Tobacco Smoke with Nitrogen Dilution Collection; CORESTA Smoke-Techno Conference, Freiburg, Germany, 2003, Presentation ST 24. Available at: https://www.coresta.org/abstracts/determination-oxides-nitrogen-mainstream-tobacco-smoke-nitrogen-dilution-collection-3934 (accessed November 2025)
Search in Google Scholar Back to article
Vincent, J., T. Mason, and I.F. Tindall: Determination of Oxides of Nitrogen (NO_x) in Analytical Smoking Part 1: Complexities in Calibration Methods; CORESTA Smoke-Techno Conference, Graz, Austria, 2011, Presentation STPOST 10. Available at: https://www.coresta.org/abstracts/determination-oxides-nitrogen-nox-analytical-smoking-part-1-comp lexities-calibration (accessed November 2025)
Search in Google Scholar Back to article
Gillman, I.G., J.D. Blomberg, I.F. Tindall, L.A. Crumpler, and J.H. Vincent: Evaluation of an Online, Puff-by-Puff Method for the Determination of Nitric Oxide, Nitrogen Dioxide, and Total Mono-Nitrogen Oxides in Fresh Mainstream Smoke; 68^th Tobacco Science Research Conference (TSRC), Charlottesville, VA, USA, 2014, Presentation 08. Available at: https://www.coresta.org/sites/default/files/abstracts/2014_TWC08_Gillman.pdf (accessed November2025)
Search in Google Scholar Back to article
Schade, K. and A. Kitta: Determination of Nitrogen Oxides in Vapour Phase of Cigarettes – Comparison of 2 Methods; CORESTA Smoke-Techno Conference, Hamburg, Germany, 2019, Presentation STPOST 21. Available at: https://www.coresta.org/sites/default/files/abstracts/2019_STPOST21_Schade.pdf (accessed November 2025)
Search in Google Scholar Back to article
Lushnikova, A.Y.: Analytical Review of Methods for the Determination of Nitrogen Oxides in Tobacco and Nicotine Containing Products; New Technologies 18 (2022) 81–86 (In Russ.). DOI: 10.47370/2072-0920-2022-18-2-81-86
Open DOI Search in Google Scholar Back to article
Cooperation Centre for Scientific Research Relative to Tobacco (CORESTA) Heated Tobacco Products Task Force: Proficiency Study for Propylene Glycol, Glycerin, Nicotine, CO, NO, NO_x, ACM, and DML in HTP Aerosol; Technical Report, September 2022. Available at: https://www.coresta.org/sites/default/files/technical_documents/main/HTP-280-CTR-ProfStudy-for-Major-Constituents-in-HTP-Aerosol_Sept2022.pdf (accessed November 2025)
Search in Google Scholar Back to article
University of Kentucky, College of Agriculture, Food and Environment, Center for Tobacco Reference Products: Certified Reference Cigarettes; Lexington, KY, USA. Available at: https://ctrp.uky.edu/home (accessed November 2025)
Search in Google Scholar Back to article
Cooperation Centre for Scientific Research Relative to Tobacco (CORESTA): CORESTA Monitors; CORESTA, Paris, France. Available at: https://www. coresta.org/coresta-monitors (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO 3402:2023 – Tobacco and Tobacco Products – Atmosphere for Conditioning and Testing; ISO, Geneva, Switzerland, Edition 5, 2023. Available at: https://www.iso.org/standard/83089.html (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO 4387:2019 – Cigarettes – Determination of Total and Nicotine-Free Dry Particulate Matter Using a Routine Analytical Smoking Machine; ISO, Geneva, Switzerland, Edition 4, 2019. Available at: https://www.iso.org/standard/76549.html (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO 20779:2018 – Cigarettes – Determination of Nicotine in Total Particulate Matter from the Mainstream Smoke – Gas-Chromatographic Method; ISO, Geneva, Switzerland, Edition 1, 2018. Available at: https://www.iso.org/standard/69066.html (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO 3308:2012 – Routine Analytical Cigarette-Smoking Machine – Definitions and Standard Conditions; ISO, Geneva, Switzerland, Edition 5, 2012. Available at: https://www.iso.org/standard/60404.html (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO 20778:2018 – Cigarettes – Routine Analytical Cigarette Smoking Machine – Definitions and Standard Conditions with an Intense Smoking Regime; ISO, Geneva, Switzerland, Edition 1, 2018. Available at: https://www.iso.org/standard/69065.html (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO/IEC 17043:2023 – Conformity Assessment – General Requirements for Proficiency Testing; ISO, Geneva, Switzerland, Edition 2, 2023. Available at: https://www.iso.org/standard/80864.html (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO 13528:2022 – Statistical Methods for Use in Proficiency Testing by Interlaboratory Comparisons; ISO, Geneva, Switzerland, Edition 3, 2022. Available at: https://www.iso.org/standard/78879.html (accessed November 2025)
Search in Google Scholar Back to article
International Organization for Standardization (ISO): ISO 5725-2:2019 – Accuracy (Trueness and Precision) of Measurement Methods and Results – Part 2: Basic Method for the Determination of Repeatability and Reproducibility of a Standard Measurement Method; ISO, Geneva, Switzerland, Edition 2, 2019. Available at: https://www.iso.org/standard/69419.html (accessed November 2025)
Search in Google Scholar Back to article
Cooperation Centre for Scientific Research Relative to Tobacco (CORESTA): 2021 Study for NO_x in Mainstream Cigarette Smoke; SA Technical Report, CORESTA, Paris, France, June 2022. Available at: https://www.coresta.org/2021-study-nox-mainstream-c igarette-smoke-36362.html (accessed November 2025)
Search in Google Scholar Back to article
Piadé, J.J., S. Wajrock, G. Jaccard, and G. Janeke: Formation of Mainstream Cigarette Smoke Constituents Prioritized by the World Health Organization – Yield Patterns Observed in Market Surveys, Clustering and Inverse Correlations; Food Chem. Toxicol. 55 (2013) 329–347. DOI: 10.1016/j.fct.2013.01.016
Open DOI Search in Google Scholar Back to article
Cooperation Centre for Scientific Research Relative to Tobacco (CORESTA): CORESTA Recommended Method N° 104 – Determination of Oxides of Nitrogen (NO_x) in Mainstream Cigarette Smoke by Chemiluminescence; CORESTA, Paris, France, August 2023. Available at: https://www.coresta.org/determination-oxides-nitrogen-nox-mainstream-cigar ette-smoke-chemiluminescence-37876.html (accessed November 2025)
Search in Google Scholar Back to article

Determination of NOx in Mainstream Cigarette Smoke, CORESTA Collaborative Study and Recommended Method

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