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Journal Details
Format
Journal
eISSN
2719-9509
First Published
01 Jan 1992
Publication timeframe
4 times per year
Languages
English

Search

Volume 29 (2020): Issue 2 (August 2020)

Journal Details
Format
Journal
eISSN
2719-9509
First Published
01 Jan 1992
Publication timeframe
4 times per year
Languages
English

Search

5 Articles
Open Access

Editors’ Note

Published Online: 25 Sep 2020
Page range: 55 - 56

Abstract

Open Access

Analysis of α-Tocopherol in Tobacco and Cigarette Smoke

Published Online: 25 Sep 2020
Page range: 57 - 65

Abstract

Summary

α-Tocopherol, a type of vitamin E, has been known to be present in tobacco for many years. The compound is an antioxidant protecting cell membranes from oxidants. α-Tocopherol is transferred from tobacco into cigarette smoke, where it is also present. Analysis of α-tocopherol has been reported in a number of studies and in various matrices including tobacco and tobacco smoke. However, no recent publication describes a method for quantitative analysis of tocopherol in tobacco and in cigarette smoke, and many methods reported from previous studies were not published and only presented at conferences or communicated in internal company publications.

The goal of this study was to quantitate α-tocopherol and, if present, α-tocopheryl acetate in tobacco and in tobacco smoke. For this analysis, an original HPLC technique was developed and is described in this report. Both UV and MS/MS (MRM mode) were used as detection procedure for the analysis. The results obtained using UV detection were in very good agreement with the results obtained using MS/MS detection. The method has been applied for the analysis of a number of tobaccos, as well as the total particulate matter (TPM) from cigarettes made with the same tobaccos. Depending on tobacco type, the levels of α-tocopherol vary in tobacco between about 200 μg/g up to about 900 μg/g (“dry weight basis”). For ISO type smoking, the levels of α-tocopherol vary in TPM between about 2 μg/mg up to slightly above 4 μg/mg of TPM. For a cigarette generating TPM of about 10 mg/cig, the α-tocopherol is between about 20 μg/cig up to about 40 μg/cig. A relatively good correlation was obtained between the level of α-tocopherol in smoke (ISO type smoking) and the level of the compound in tobacco. α-Tocopheryl acetate was absent in tobacco.

Keywords

  • α-Tocopherol
  • α-tocopheryl acetate
  • tobacco
  • cigarette smoke
Open Access

Robustness of HPHC Reduction for THS 2.2 Aerosol Compared with 3R4F Reference Cigarette Smoke Under High Intensity Puffing Conditions

Published Online: 25 Sep 2020
Page range: 66 - 83

Abstract

Summary

In the absence of standards specific for testing the reduction robustness of the levels of harmful and potentially harmful constituents (HPHCs), the aerosol from the THS 2.2, a heated tobacco product, was compared with the mainstream smoke of the 3R4F reference cigarette over a broad range of machine-smoking regimes. The average reduction and the introduced concept of threshold limits of robust reduction were derived from HPHC concentrations, in mass per tobacco-stick normalized per total puff volume, to propose an alternative for the assessment of products where nicotine-adjusted yields would be inappropriate. In addition, this study explores the influence of 3R4F reference cigarette filter ventilation, and discusses the roles of temperature and precursors in the present context of robustness of HPHC reduction. Fifty-four HPHCs were analyzed under multiple regimes in THS 2.2 aerosol and 3R4F cigarette smoke. The average reduction of HPHC concentrations compared across all regimes characterized the robustness. Threshold limits of reduction of individual HPHCs were statistically determined across all regimes. The results observed under Health Canada Intense (HCI) and more intense regimes indicated that on average the reductions in HPHCs levels investigated in THS 2.2 aerosol were more than 90% and that the majority of the 54 HPHCs investigated in THS 2.2 aerosol showed more than 90% reduction. The robustness of THS 2.2 in maintaining the levels of reduction of representative HPHCs, whatever the puffing regime, can be quantified. The mass of HPHC per tobacco-stick normalized per total puff volume is a valuable approach to compare the robustness of the performance of a product over a large range of puffing conditions. Our findings will greatly complement the assessment for robustness of current and future similar products where classical approaches would present limitations.

Keywords

  • Tobacco Heating System
  • THS 2.2
  • reduced-risk product
  • harmful and potentially harmful constituent
  • HPHC
  • aerosol chemistry
Open Access

Variations of TSNA Levels in Tobaccos Upon Heating at Moderate Temperatures

Published Online: 25 Sep 2020
Page range: 84 - 96

Abstract

Summary

Tobacco-specific nitrosamines (TSNAs) including nitrosoanabasine (NAB), nitrosoanatabine (NAT), 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), and nitrosonornicotine (NNN) are naturally present at trace levels in tobacco. During tobacco processing, preparation of expanded tobacco, and when tobacco is used in heat-not-burn type cigarettes, the tobacco is exposed to different degrees of heat. Heating of tobacco has been reported in the literature to increase the level of TSNAs. Since the increase of TSNAs in heated tobacco is still not well understood, the present study evaluated TSNA levels in six types of tobacco as a function of moderate heat exposure. These tobaccos included: flue-cured lower stalk, flue-cured upper stalk (US), Burley lower stalk, Burley upper stalk (US), and two Oriental blends (Turkey, Greece, Bulgaria, Northern Republic Macedonia). Heating was performed in sealed glass tubes at oven temperatures of 100 °C, 150 °C, 200 °C, and 250 °C for time intervals of 2 min and 5 min. The temperatures inside the glass tubes were lower than the targets and were monitored separately as a function of glass tube heating. The study showed no meaningful differences within tobacco type (by stalk position) but showed considerable differences in the levels of TSNAs between different tobaccos, with the Burley tobaccos having the highest levels, and the Orientals the lowest. For all tobacco types, TSNAs increase to some extent when temperature increases. For 2-min heating, the increase in TSNAs is relatively small up to about 200 °C, but the levels almost double when the oven temperature increases to 250 °C. For 5-min heating, the increase in TSNAs starts at about 150 °C with a maximum at 200 °C which can reach more than double the initial TSNA level. Longer heating at 250 °C (5 min) starts to cause TSNAs decomposition and the levels are reduced.

Keywords

  • TSNAs
  • tobacco heating
  • moderate temperatures
Open Access

Statistical Analysis for Comparison of the Results Obtained by Capillary Columns and Packed Columns in the Determination of Water Yield in Smoke Condensates Analyzed in Cigarettes for the 24th Asia Collaborative Study

Published Online: 25 Sep 2020
Page range: 97 - 118

Abstract

Summary

Recently, capillary columns have been widely used in the methodology for the determination of water yields in smoke condensate, even though ISO 10362-1:1999, “Cigarettes - Determination of water in smoke condensates – Part 1: Gas chromatographic method” specifies a packed gas chromatographic column. As a result of a systematic review in 2015, ISO/TC126 decided to revise the standard to include the use of capillary columns.

The goal of this study was to confirm the comparability of water yields obtained from capillary column methodology to those yields from packed columns by the statistical analysis of yield data from the 24th Asia Collaborative Study which included 86 datasets submitted by 64 laboratories. After the exclusion of outliers by Cochran’s and Grubbs’ tests, the datasets were classified by GC column type and then mean water yields, and their repeatability and reproducibility were calculated for each type of column. No significant differences were observed in water yields between capillary and packed columns. Repeatability and reproducibility of water yields using capillary column were comparable to those using packed columns as described in ISO 10362-1:1999. From these results, it was confirmed that the capillary columns are an appropriate alternative to packed columns for the gas chromatographic procedure described in ISO 10362-1:1999.

5 Articles
Open Access

Editors’ Note

Published Online: 25 Sep 2020
Page range: 55 - 56

Abstract

Open Access

Analysis of α-Tocopherol in Tobacco and Cigarette Smoke

Published Online: 25 Sep 2020
Page range: 57 - 65

Abstract

Summary

α-Tocopherol, a type of vitamin E, has been known to be present in tobacco for many years. The compound is an antioxidant protecting cell membranes from oxidants. α-Tocopherol is transferred from tobacco into cigarette smoke, where it is also present. Analysis of α-tocopherol has been reported in a number of studies and in various matrices including tobacco and tobacco smoke. However, no recent publication describes a method for quantitative analysis of tocopherol in tobacco and in cigarette smoke, and many methods reported from previous studies were not published and only presented at conferences or communicated in internal company publications.

The goal of this study was to quantitate α-tocopherol and, if present, α-tocopheryl acetate in tobacco and in tobacco smoke. For this analysis, an original HPLC technique was developed and is described in this report. Both UV and MS/MS (MRM mode) were used as detection procedure for the analysis. The results obtained using UV detection were in very good agreement with the results obtained using MS/MS detection. The method has been applied for the analysis of a number of tobaccos, as well as the total particulate matter (TPM) from cigarettes made with the same tobaccos. Depending on tobacco type, the levels of α-tocopherol vary in tobacco between about 200 μg/g up to about 900 μg/g (“dry weight basis”). For ISO type smoking, the levels of α-tocopherol vary in TPM between about 2 μg/mg up to slightly above 4 μg/mg of TPM. For a cigarette generating TPM of about 10 mg/cig, the α-tocopherol is between about 20 μg/cig up to about 40 μg/cig. A relatively good correlation was obtained between the level of α-tocopherol in smoke (ISO type smoking) and the level of the compound in tobacco. α-Tocopheryl acetate was absent in tobacco.

Keywords

  • α-Tocopherol
  • α-tocopheryl acetate
  • tobacco
  • cigarette smoke
Open Access

Robustness of HPHC Reduction for THS 2.2 Aerosol Compared with 3R4F Reference Cigarette Smoke Under High Intensity Puffing Conditions

Published Online: 25 Sep 2020
Page range: 66 - 83

Abstract

Summary

In the absence of standards specific for testing the reduction robustness of the levels of harmful and potentially harmful constituents (HPHCs), the aerosol from the THS 2.2, a heated tobacco product, was compared with the mainstream smoke of the 3R4F reference cigarette over a broad range of machine-smoking regimes. The average reduction and the introduced concept of threshold limits of robust reduction were derived from HPHC concentrations, in mass per tobacco-stick normalized per total puff volume, to propose an alternative for the assessment of products where nicotine-adjusted yields would be inappropriate. In addition, this study explores the influence of 3R4F reference cigarette filter ventilation, and discusses the roles of temperature and precursors in the present context of robustness of HPHC reduction. Fifty-four HPHCs were analyzed under multiple regimes in THS 2.2 aerosol and 3R4F cigarette smoke. The average reduction of HPHC concentrations compared across all regimes characterized the robustness. Threshold limits of reduction of individual HPHCs were statistically determined across all regimes. The results observed under Health Canada Intense (HCI) and more intense regimes indicated that on average the reductions in HPHCs levels investigated in THS 2.2 aerosol were more than 90% and that the majority of the 54 HPHCs investigated in THS 2.2 aerosol showed more than 90% reduction. The robustness of THS 2.2 in maintaining the levels of reduction of representative HPHCs, whatever the puffing regime, can be quantified. The mass of HPHC per tobacco-stick normalized per total puff volume is a valuable approach to compare the robustness of the performance of a product over a large range of puffing conditions. Our findings will greatly complement the assessment for robustness of current and future similar products where classical approaches would present limitations.

Keywords

  • Tobacco Heating System
  • THS 2.2
  • reduced-risk product
  • harmful and potentially harmful constituent
  • HPHC
  • aerosol chemistry
Open Access

Variations of TSNA Levels in Tobaccos Upon Heating at Moderate Temperatures

Published Online: 25 Sep 2020
Page range: 84 - 96

Abstract

Summary

Tobacco-specific nitrosamines (TSNAs) including nitrosoanabasine (NAB), nitrosoanatabine (NAT), 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), and nitrosonornicotine (NNN) are naturally present at trace levels in tobacco. During tobacco processing, preparation of expanded tobacco, and when tobacco is used in heat-not-burn type cigarettes, the tobacco is exposed to different degrees of heat. Heating of tobacco has been reported in the literature to increase the level of TSNAs. Since the increase of TSNAs in heated tobacco is still not well understood, the present study evaluated TSNA levels in six types of tobacco as a function of moderate heat exposure. These tobaccos included: flue-cured lower stalk, flue-cured upper stalk (US), Burley lower stalk, Burley upper stalk (US), and two Oriental blends (Turkey, Greece, Bulgaria, Northern Republic Macedonia). Heating was performed in sealed glass tubes at oven temperatures of 100 °C, 150 °C, 200 °C, and 250 °C for time intervals of 2 min and 5 min. The temperatures inside the glass tubes were lower than the targets and were monitored separately as a function of glass tube heating. The study showed no meaningful differences within tobacco type (by stalk position) but showed considerable differences in the levels of TSNAs between different tobaccos, with the Burley tobaccos having the highest levels, and the Orientals the lowest. For all tobacco types, TSNAs increase to some extent when temperature increases. For 2-min heating, the increase in TSNAs is relatively small up to about 200 °C, but the levels almost double when the oven temperature increases to 250 °C. For 5-min heating, the increase in TSNAs starts at about 150 °C with a maximum at 200 °C which can reach more than double the initial TSNA level. Longer heating at 250 °C (5 min) starts to cause TSNAs decomposition and the levels are reduced.

Keywords

  • TSNAs
  • tobacco heating
  • moderate temperatures
Open Access

Statistical Analysis for Comparison of the Results Obtained by Capillary Columns and Packed Columns in the Determination of Water Yield in Smoke Condensates Analyzed in Cigarettes for the 24th Asia Collaborative Study

Published Online: 25 Sep 2020
Page range: 97 - 118

Abstract

Summary

Recently, capillary columns have been widely used in the methodology for the determination of water yields in smoke condensate, even though ISO 10362-1:1999, “Cigarettes - Determination of water in smoke condensates – Part 1: Gas chromatographic method” specifies a packed gas chromatographic column. As a result of a systematic review in 2015, ISO/TC126 decided to revise the standard to include the use of capillary columns.

The goal of this study was to confirm the comparability of water yields obtained from capillary column methodology to those yields from packed columns by the statistical analysis of yield data from the 24th Asia Collaborative Study which included 86 datasets submitted by 64 laboratories. After the exclusion of outliers by Cochran’s and Grubbs’ tests, the datasets were classified by GC column type and then mean water yields, and their repeatability and reproducibility were calculated for each type of column. No significant differences were observed in water yields between capillary and packed columns. Repeatability and reproducibility of water yields using capillary column were comparable to those using packed columns as described in ISO 10362-1:1999. From these results, it was confirmed that the capillary columns are an appropriate alternative to packed columns for the gas chromatographic procedure described in ISO 10362-1:1999.

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