Variation in Smoke Toxicant Yields from Selected Cigarettes

Transcription

1 Variation in Smoke Toxicant Yields from Selected Cigarettes lison Eldridge (SSPT), Tatiana Betson (P), Kevin Mcdam 2013 COREST Joint Study Group Meetings SSPT Seville, Spain / 29 Sept - 3 Oct P Brufa di Torgiano, Italy / Oct

2 Background The WHO, through the TobReg study group, have proposed the regulation of toxicant emissions from cigarette mainstream smoke - 9 toxicants (TobReg9) are recommended for mandated lowering n understanding of variation is required in order to contextualise the toxicant measurement data. Designed a study to provide data on variability in toxicant emissions WHO World Health Organisation TobReg The WHO Study Group on Tobacco Product Regulation

3 Study Design To understand how representative is a sample of commercial cigarettes taken at a single time-point 3 high volume commercial cigarettes from a single market - 2 x BT products (10mg & 4mg ISO tar yield) - 1 product by another manufacturer (10mg ISO tar yield) - Sampled monthly for 10 consecutive months - ugust 2010 to May 2011 Laboratory control 3R4F nalyses conducted at single BT laboratory - Full Hoffmann suite at both HCI and ISO regimes - Cigarette filler blend - Cigarette physical measurements Focus on TobReg9 toxicants plus nicotine at the Health Canada Intense (HCI) smoking regime

4 Data nalysis Real world approach - Did not control analysis schedule - Generally the 3 commercial products from a single month were analysed in the same analytical batch - 7 to 10 analysis batches per product per analysis - Each analysis batch included a 3R4F sample - The reported mean, of 5 replicates, per sample was used in this analysis Results investigated using summary statistics - Coefficient of Variation (CV) - Comparing within and between products - Standard Deviation (SD) - Empirical rule 2 x SD = ~95% of a normal distribution - n estimate of within laboratory tolerance around a single measured value

5 General Variation Mean CV for the 3 commercial products Generally low variation Expressing as a nicotine ratio increases variation by ~1-2% Sources of variation - nalytical - Product HPHC Nicotine Ratio CV (%)* bsolute Value CV (%)* Nicotine mg/cig 3.7 CO mg/cig ,3-Butadiene µg/cig Benzene µg/cig NNN ng/cig NNK ng/cig Formaldehyde µg/cig cetaldehdye µg/cig crolein µg/cig Benzo[a]pyrene ng/cig * Mean CV for the 3 commercial products

6 nalytical Variation Sample Preparation Smoke sample preparation Practical lower limit of variation for a reasonably controlled analysis: typically 3 6% CV for TPM

7 nalytical Variation nalytical Methods Grouped by analytical method Factors affecting variability of an analytical method - mount of toxicant - Complexity of analysis TSN analysis was the most variable 1,3-Butadiene and formaldehyde have noticeably greater variation within analysis suite HPHC Nicotine Ratio CV (%)* bsolute Value CV (%)* Nicotine mg/cig 3.7 CO mg/cig ,3-Butadiene µg/cig Benzene µg/cig NNN ng/cig NNK ng/cig Formaldehyde µg/cig cetaldehdye µg/cig crolein µg/cig Benzo[a]pyrene ng/cig * Mean CV for the 3 commercial products

8 nalytical Variation: Volatiles nalysis at HCI 1,3- Butadiene (µg/cig) B C 3R4F D B E 1,3-Butadiene F G H B nalysis Batch C D Both toxicants from the same analysis and at a similar level 1,3-butadiene clearly more variable (20.9% vs 6.1% CV) Synchronous pattern across all 4 products indicative of analytical variability Potential for improvement in analytical method - Sample collection or detection? C E F G H Benzene (µg/cig) B C 3R4F D B E F Benzene G H B nalysis Batch C D C E F G H

9 Product Variation Differences between products variation in blend composition and design - Compare absolute levels of toxicant Sources of variation within a product - product design (constant) - blend composition (recipe constant but natural tobacco variability) - manufacturing batch (variation between manufacturing runs) Effect of manufacturing batches within products by comparing variation in - 3R4F (single manufactured batch) - commercial products (multiple manufacturing batches)

10 NNN Product Variation ug-10 Sep-10 Oct-10 Nov-10 Dec-10 Jan-11 Feb-11 Mar-11 pr-11 May-11 ug-10 Sep-10 Oct-10 Nov-10 Dec-10 Jan-11 Feb-11 Mar-11 pr-11 May NNN in Blend NNN in Smoke HCI 3R4F B C R4F B C NNN ug-10 Sep-10 Oct-10 Nov-10 Dec-10 Jan-11 Feb-11 Mar-11 pr-11 May-11 ug-10 Sep-10 Oct-10 Nov-10 Dec-10 Jan-11 Feb-11 Mar-11 pr-11 May-11 Month Month * NNN data normalised to mean per product 3R4F from a single manufacturing batch Transfer of blend NNN to smoke NNN - Similar patterns of variation within a product. - Especially where product variation is greater than analytical variation

11 Product Variation: Effect of manufacturing batch Comparing Commercial products - multiple manufacturing batches to 3R4F - Single batch ratio >1 may indicate measureable manufacturing batch variability. Low ratio for 1,3- butadiene due to strong presence of analytical variability. Toxicant Coefficients of Variation (%) Commercial Products Ratio to Nicotine 3R4F Control Ratio* Commercial Products bsolute Values 3R4F Control Ratio* Nicotine CO ,3-Butadiene Benzene NNN NNK Formaldehyde cetaldehdye crolein Benzo[a]pyrene * Commercial Products / 3R4F

12 Product Variation: Uncertainty verage values for the 3 commercial products Empirically 2 x SD = ~95% of a normal distribution Suggests the range of values which might be reported for a single large volume commercial product over time in one lab Toxicant Units Mean Ratio to Nicotine bsolute Values 2xSD 2xCV(%) Mean 2xSD 2xCV(%) Nicotine mg/cig CO mg/cig ,3-Butadiene µg/cig Benzene µg/cig NNN ng/cig NNK ng/cig Formaldehyde µg/cig cetaldehdye µg/cig crolein µg/cig Benzo[a]pyrene ng/cig This kind of variability has been recognised for TNCO regulatory reporting under ISO where a tolerance of ± 15% applies for tar and nicotine +/- 20% for CO with repeated sampling

13 Conclusions We have investigated variability in toxicant emissions of three high volume commercial cigarette products. Generally variability was low at <15% CV (often < 10% CV) nalytical variability - Several toxicants showed relatively high levels of analytical variability, which may indicate a potential for analytical improvement - 1,3-Butadiene and formaldehyde - TSN was the most variable analysis Product variability - Described the variability in products and the effect of different manufacturing batches. Together these demonstrate that measurement of toxicant emissions from commercial cigarette products is associated with significant levels of variation. - This would naturally increase if measurement was conducted in more than one laboratory.