Smoking cigarettes is a cause of serious diseases in smokers including lung cancer, heart disease, and emphysema. Phenolic compounds catechol, hydroquinone, resorcinol, phenol, and/or
Phenols have been measured by various methods at least since the 1960s for research, product characterization, and selective filtration purposes (6–13). In particular, Health Canada’s T-114 was treated as a starting point for the study reported here (14). The scope of T-114 is limited to phenolic determination using intense smoking regime T-115 (15). The purpose of this study was to establish a method with a broader scope and to establish repeatability and reproducibility estimates for the determination of phenolic compounds using cigarettes and test pieces across a wide range of “tar” yield and cigarette designs.
Thus, a collaborative study was conducted involving 20 laboratories from 11 countries, smoking 10 samples from the world-wide market. The samples had a range of blend styles (Virginia, American blend, and dark air-cured) and ISO 3308 “tar” yields between 1 and 13 mg. The cigarettes were smoked under both the ISO 3308 and ISO 20778 smoking regimes (16–17).
Statistical evaluations were made according to ISO 5725 recommendations and repeatability and reproducibility data are provided (18).
The laboratories that conducted the testing along with the product volunteers are listed in alphabetical order in Table 1. To ensure anonymity of the results, each laboratory was given a unique study code for data exchange and reporting.
Participating laboratories and product volunteers.
Testing participants | |
---|---|
Altria Client Services | ITC Ltd. |
ARISTA Laboratories | ITG, France |
BAT Souza Cruz SA – Brazil | ITL – Reemtsma Cigarettenfabriken |
British American Tobacco | Japan Tobacco Inc. |
China National Tobacco Corp. Beijing Cigarette Factory | Japan Tobacco International |
CNTC – Zhengzhou Tobacco Research Institute | KT&G Corp. |
CNTC QC | Labstat International Inc. |
Enthalpy Analytical, Inc. | Philip Morris International – Brazil |
Essentra Scientific Services | Philip Morris International – Indonesia |
Global Laboratory Services, Inc. | R.J. Reynolds Tobacco Co. |
Product Volunteers | |
---|---|
British American Tobacco Germany GmbH | Japan Tobacco – Japan |
China National Tobacco Corp. Beijing Cigarette Factory | Philip Morris International – Neuchatel, Switzerland |
ITG Altadis | Shanghai Tobacco Group Co. Ltd |
Participating laboratories were asked to follow a supplied study protocol, a draft of a CORESTA Recommended Method (CRM), and Health Canada T-114 (14) analytical method for the determination of phenols. Samples analyzed for the study are listed in Table 2 with a range of blend and cigarette designs that represent the market and a wide range of total particulate matter (TPM) and analyte yields. In accordance with the study protocol, participating laboratories were asked to obtain reference cigarettes and monitor test pieces directly from suppliers (19–20). Other samples were commercial products from various regions provided by the study volunteers listed in Table 1. Five replicates of each product with each smoking regime were requested to be generated. Reportable measures included puff count, TPM, hydroquinone, resorcinol, catechol, phenol,
Study samples.
Sample ID | Blend description | Approximate TPM ISO 3308 regime (mg/cig)a | Approximate TPM ISO 20778 regime (mg/cig) |
---|---|---|---|
CM7 | Virginia | 16.1 | 43.4 |
KR 1R5F | American | 2.0 | 31.8 |
KR 3R4F | American | 9.9 | 44.1 |
Sample 1 | Dark air-cured | 13.5 | 44.1 |
Sample 2 | American | 8.9 | 40.2 |
Sample 3 | American | 10.2 | 45.1 |
Sample 4 | Virginia | 4.0 | 30.3 |
Sample 5 | Virginia | 1.8 | 20.6 |
Sample 6 | Virginia | 11.3 | 36.1 |
Sample 7 | Charcoal filtered | 1.2 | 25.8 |
Based on the average TPM values from the study reported in this report
The yields of phenols collected under ISO 3308 (non-intense) and ISO 20778 (intense) smoking regimes were reported in units of microgram per cigarette (µg/cig) in the templates provided to participants.
Following the recommended method, conditioned cigarettes were smoked using an automated 20-port constant volume smoking machine, onto a conditioned, pre-weighed glass fiber filter disc (pad).
TPM was determined gravimetrically and puff counts were as recorded. The pads were extracted using 40 mL of 1% aqueous acetic acid with 30 min of agitation using a wrist-action shaker. Extracts were diluted using 1% acetic acid based on total TPM. Samples below 15 mg TPM were tested undiluted. Samples with 15–60 mg TPM were diluted 2:5 and samples with 60–100 mg TPM were diluted 1:5 prior to analysis.
Samples were analyzed within 24 hours of collection and extraction as hydroquinone is subject to rapid oxidation. Samples were analyzed using high performance liquid chromatography with selective fluorescence detection (HPLC-FLD).
Detector settings are included in Table 3.
Fluorescence detector settings.
Time initial | Excitation (nm) | Emission (nm) |
---|---|---|
0.0 | 280 | 310 |
12.4 | 280 | 310 |
12.5 | 274 | 298 |
23.0 | 274 | 298 |
24.0 | 280 | 310 |
28.0 | 280 | 310 |
The mobile phase consisted of: 1% acetic acid (HOAC) (aqueous; solvent A); 1% HOAC (in methanol; solvent B) with a flow rate of 0.8 mL/min and an elution gradient as noted in Table 4.
Elution program.a
Time (min) | Composition | |
---|---|---|
% A | % B | |
0 | 78 | 22 |
8 | 78 | 22 |
8.5 | 55 | 45 |
21 | 55 | 45 |
22 | 0 | 100 |
28 | 0 | 100 |
(Equilibrate 6 min) |
Linear gradient
Sample injection volume was 10 µL to 20 µL onto a pentafluorophenylpropyl analytical column (4.6 mm × 150 mm × 3 µm).
Data consistency was verified using graphical and numerical outlier detection techniques. Mandel’s
Mandel’s
Straggling data were retained in the dataset but outlying data were removed for descriptive statistics reporting. Overall mean, standard deviation, repeatability (r), and reproducibility (R) values were determined according to ISO 5725-216 (18).
The study design allowed for evaluation of the robustness of the method across the linear range for analytes of interest and confirmed the method’s effectiveness with a variety of products.
Thus, the study samples chosen represented a wide variety of TPM yields, tobacco blends, and product construction parameters including varied filter ventilation level and inclusion of a filter additive for one study sample. Non-intense and intense smoking regimes were used to verify applicability with the recommended method.
Smoking related measures, including puff count and TPM, had low variability for both smoking regimes and across all products. Sample 7 (activated charcoal filter and high filter ventilation) showed the highest variability among the products tested. Additionally, no significant differences in results were noted based on choice of smoking machine type (i.e., linear or rotary). The method appears to distinguish samples appropriately. As expected of particulate phase and pad-trapped semi-volatile constituents, the analyte yields were directly correlated to TPM yields. When normalized to TPM, phenols showed predictable trending based on blend type. For example, Virginia (i.e., fluecured) products had higher phenolic:TPM values compared to American blend samples containing Burley tobacco.
In general, CM7 had the highest phenolic:TPM values. This is consistent with previous research indicating that flue-cured tobacco may generate higher levels of some phenolic HPHCs (10, 21).
Several data sets included non-numeric (i.e., < LOQ) reporting for resorcinol, phenol, and the cresol compounds. These values were excluded from outlier evaluation and calculation of descriptive statistics and repeatability (r), and reproducibility (R) values.
Results of graphical outlier detection methods (Mandel’s
Mean, r, and R results with outliers removed are displayed in Table 5 and Table 6. Values are typically above limits established in ISO 8243 (22) for “tar”, nicotine, and carbon monoxide (TNCO). This is not unexpected given the much lower levels for phenols (µg) than TNCO measures (mg). Additionally, the highest values for r and R noted in the study were for results near LOQ at limits of the method’s capabilities.
Non-intense smoking regime – Inter-laboratory mean yields, repeatability (r) and reproducibility (R) data.
CM7 | 1R5F | 3R4F | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | ||
---|---|---|---|---|---|---|---|---|---|---|---|
Puff count | Mean a | 8.45 | 6.90 | 8.28 | 5.66 | 7.88 | 6.91 | 5.19 | 4.54 | 6.82 | 6.16 |
STD b | 0.35 | 0.27 | 0.33 | 0.27 | 0.36 | 0.34 | 2.35 | 1.10 | 1.65 | 0.25 | |
TPM | Mean | 16.12 | 1.96 | 9.85 | 13.46 | 8.85 | 10.24 | 3.26 | 1.69 | 10.64 | 1.17 |
STD | 1.07 | 0.32 | 0.78 | 1.78 | 0.75 | 0.84 | 1.71 | 0.52 | 2.90 | 0.31 | |
Hydroquinone | Mean | 91.82 | 8.45 | 32.84 | 42.78 | 36.98 | 46.88 | 20.38 * | 9.30 | 46.69 | 8.09 |
STD | 7.47 | 1.33 | 2.78 | 3.85 | 3.43 | 3.60 | 3.26 | 1.19 | 4.08 | 0.96 | |
r c | 12.14 | 1.58 | 4.27 | 8.92 | 5.97 | 6.72 | 2.89 | 1.78 | 6.31 | 1.41 | |
R d | 23.58 | 3.97 | 8.67 | 13.40 | 10.99 | 11.75 | 9.49 | 3.68 | 12.73 | 2.97 | |
N e | 18 | 17 | 18 | 14 | 18 | 18 | 14 | 18 | 16 | 18 | |
Resorcinol | Mean | 1.79 * | 0.13 * | 0.63 * | 0.66 * | 0.80 * | 0.97 * | 0.51 | 0.35 | 1.19 * | 0.12 * |
STD | 0.30 | 0.04 | 0.15 | 0.21 | 0.16 | 0.18 | 0.09 | 0.05 | 0.21 | 0.03 * | |
r | 0.52 | 0.09 | 0.19 | 0.37 | 0.29 | 0.29 | 0.18 | 0.14 | 0.22 | 0.10 | |
R | 0.95 | 0.14 | 0.46 | 0.67 | 0.51 | 0.58 | 0.30 | 0.17 | 0.63 | 0.13 | |
N | 17 | 13 | 15 | 12 | 16 | 16 | 13 | 15 | 15 | 12 | |
Catechol | Mean | 96.39 | 8.13 | 36.77 | 35.30 | 39.87 | 42.61 | 24.17 | 12.89 | 58.19 | 7.84 |
STD | 4.13 | 0.62 | 1.72 | 1.53 | 2.45 | 2.16 | 2.41 | 0.68 | 3.09 | 0.59 | |
r | 13.39 | 1.60 | 5.02 | 7.32 | 6.84 | 4.91 | 4.77 | 1.98 | 7.58 | 1.88 | |
R | 16.65 | 2.25 | 6.60 | 7.83 | 9.19 | 7.46 | 7.99 | 2.61 | 11.00 | 2.35 | |
N | 18 | 17 | 18 | 14 | 18 | 17 | 15 | 18 | 16 | 18 | |
Phenol | Mean | 27.60 * | 0.93 | 7.06 | 19.97 | 9.64 | 12.47 | 4.58 | 1.21 * | 13.91 | 0.49 * |
STD | 2.94 | 0.19 | 0.80 | 1.49 | 1.28 | 1.15 | 1.11 | 0.25 | 1.42 | 0.11 | |
r | 4.17 | 0.44 | 1.59 | 4.12 | 2.43 | 2.52 | 1.24 | 0.36 | 3.04 | 0.29 | |
R | 9.05 | 0.65 | 2.64 | 5.57 | 4.20 | 3.93 | 3.30 | 0.77 | 4.81 | 0.39 | |
N | 16 | 14 | 18 | 14 | 18 | 18 | 15 | 16 | 16 | 13 | |
Mean | 5.63 | 0.38 | 2.33 | 5.75 | 2.62 | 3.30 | 1.34 | 0.42 * | 3.40 | 0.21 | |
STD | 0.68 | 0.08 | 0.27 | 0.65 | 0.37 | 0.35 | 0.26 | 0.10 | 0.43 | 0.07 | |
r | 0.96 | 0.15 | 0.54 | 1.22 | 0.63 | 0.67 | 0.29 | 0.15 | 0.66 | 0.12 | |
R | 2.08 | 0.25 | 0.90 | 2.11 | 1.18 | 1.14 | 0.78 | 0.31 | 1.35 | 0.23 | |
N | 18 | 15 | 18 | 14 | 18 | 18 | 15 | 16 | 16 | 13 | |
Mean | 4.57 | 0.32 | 1.83 | 3.73 | 2.03 | 2.50 | 1.10 | 0.38 | 2.78 | 0.24 | |
STD | 0.67 | 0.10 | 0.18 | 0.45 | 0.33 | 0.29 | 0.22 | 0.07 | 0.28 | 0.12 | |
r | 0.69 | 0.12 | 0.37 | 0.77 | 0.42 | 0.43 | 0.23 | 0.11 | 0.53 | 0.10 | |
R | 1.98 | 0.29 | 0.61 | 1.43 | 0.99 | 0.90 | 0.64 | 0.23 | 0.92 | 0.36 | |
N | 17 | 13 | 17 | 13 | 17 | 17 | 14 | 17 | 16 | 13 | |
Mean | 12.45 | 0.73 | 4.56 | 10.40 | 5.44 | 6.49 | 2.49 | 0.88 | 6.25 | 0.44 | |
STD | 1.24 | 0.14 | 0.51 | 0.87 | 0.71 | 0.60 | 0.50 | 0.13 | 0.73 | 0.13 | |
r | 1.63 | 0.27 | 0.75 | 2.24 | 1.19 | 1.07 | 0.47 | 0.20 | 1.02 | 0.16 | |
R | 3.76 | 0.46 | 1.58 | 3.16 | 2.26 | 1.93 | 1.47 | 0.40 | 2.24 | 0.39 | |
N | 17 | 16 | 17 | 13 | 17 | 17 | 14 | 17 | 16 | 17 |
Mean: mean yield (μg/cig) except TPM (mg/cig) and puff count (pc)
STD: overall standard deviation
r: repeatability (μg/cig at 95% confidence interval)
R: reproducibility (μg/cig at 95% confidence interval)
N: number of datasets used for r and R determination after removal of outliers and non-quantifiable values
Values calculated after removal of outlier (s)
Intense smoking regime – Inter-laboratory mean yields, repeatability (r) and reproducibility (R) data.
CM7 | 1R5F | 3R4F | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | ||
---|---|---|---|---|---|---|---|---|---|---|---|
Puff count | Mean a | 11.78 | 6.40 | 10.39 | 7.00 | 9.74 | 7.62 | 5.81 | 5.02 | 9.31 | 6.54 |
STD b | 0.56 | 0.36 | 0.51 | 0.40 | 0.51 | 0.52 | 2.63 | 1.25 | 2.33 | 0.37 | |
TPM | Mean | 43.36 | 31.83 | 44.12 | 44.11 | 40.16 | 45.09 | 24.62 | 19.43 | 33.86 | 25.79 |
STD | 6.09 | 4.07 | 3.97 | 4.80 | 4.62 | 4.87 | 12.32 | 5.91 | 9.33 | 3.76 | |
Hydroquinone | Mean | 191.17 | 53.41 | 89.62 | 91.44 | 101.85 | 114.04 | 76.44 * | 43.56 | 106.50 | 60.19 |
STD | 15.16 | 5.08 | 7.49 | 7.99 | 8.60 | 6.30 | 5.32 | 4.30 | 9.49 | 5.47 | |
r c | 27.40 | 11.85 | 11.67 | 18.19 | 15.75 | 18.27 | 9.98 | 9.36 | 15.97 | 17.18 | |
R d | 49.02 | 17.74 | 23.43 | 27.67 | 27.88 | 24.05 | 17.37 | 14.67 | 30.16 | 21.70 | |
N e | 18 | 17 | 18 | 14 | 18 | 18 | 14 | 18 | 16 | 18 | |
Resorcinol | Mean | 3.77 | 1.07 * | 1.87 * | 1.35 * | 2.55 | 2.77 | 2.21 | 2.07 | 2.70 | 1.46 |
STD | 0.79 | 0.15 | 0.40 | 0.41 | 0.68 | 0.79 | 0.48 | 0.44 | 0.39 | 0.42 | |
r | 0.70 | 0.38 | 0.45 | 0.60 | 0.65 | 0.75 | 0.80 | 0.68 | 0.71 | 0.57 | |
R | 2.31 | 0.55 | 1.18 | 1.27 | 1.99 | 2.32 | 1.52 | 1.39 | 1.26 | 1.27 | |
N | 18 | 14 | 15 | 11 | 17 | 18 | 15 | 17 | 16 | 17 | |
Catechol | Mean | 198.81 | 41.73 | 90.24 | 76.29 | 100.18 | 96.21 | 79.79 * | 54.38 | 127.00 * | 51.10 |
STD | 15.11 | 3.55 | 6.71 | 6.52 | 7.92 | 9.10 | 6.22 | 4.56 | 6.48 | 5.27 | |
r | 27.35 | 9.81 | 14.58 | 14.03 | 14.46 | 20.19 | 11.53 | 12.81 | 24.78 | 13.13 | |
R | 48.87 | 13.26 | 22.87 | 22.16 | 25.68 | 31.23 | 20.24 | 17.16 | 28.64 | 18.86 | |
N | 18 | 17 | 18 | 14 | 18 | 18 | 14 | 18 | 15 | 18 | |
Phenol | Mean | 43.05 | 8.20 | 13.13 | 36.65 | 16.99 | 19.19 | 12.00 | 6.64 | 19.33 * | 6.93 |
STD | 3.59 | 0.91 | 1.05 | 1.20 | 1.46 | 1.59 | 1.33 | 0.63 | 1.35 | 0.57 | |
r | 8.93 | 1.88 | 3.30 | 8.39 | 4.14 | 4.82 | 2.96 | 1.74 | 4.59 | 3.13 | |
R | 12.83 | 3.05 | 4.17 | 8.22 | 5.51 | 6.21 | 4.56 | 2.34 | 5.58 | 3.23 | |
N | 18 | 17 | 18 | 14 | 18 | 18 | 15 | 18 | 15 | 18 | |
Mean | 8.67 | 2.53 | 4.15 | 10.88 | 4.66 | 5.22 | 3.14 * | 1.90 | 4.53 * | 1.97 | |
STD | 1.14 | 0.28 | 0.50 | 0.99 | 0.60 | 0.60 | 0.38 | 0.22 | 0.41 | 0.28 | |
r | 1.89 | 0.58 | 0.96 | 2.52 | 1.05 | 1.22 | 0.66 | 0.52 | 1.15 | 0.91 | |
R | 3.62 | 0.93 | 1.64 | 3.58 | 1.93 | 2.01 | 1.22 | 0.78 | 1.55 | 1.13 | |
N | 18 | 16 | 18 | 14 | 18 | 18 | 14 | 17 | 15 | 17 | |
Mean | 7.08 | 1.78 | 3.25 | 7.14 | 3.58 | 3.90 | 2.65 | 1.58 | 3.91 | 1.67 | |
STD | 1.07 | 0.22 | 0.45 | 0.74 | 0.51 | 0.37 | 0.43 | 0.22 | 0.37 | 0.35 | |
r | 1.27 | 0.48 | 0.72 | 1.49 | 0.68 | 0.90 | 0.64 | 0.45 | 0.84 | 0.69 | |
R | 3.22 | 0.76 | 1.42 | 2.47 | 1.55 | 1.31 | 1.34 | 0.74 | 1.28 | 1.16 | |
N | 17 | 16 | 17 | 13 | 17 | 16 | 14 | 17 | 16 | 17 | |
Mean | 20.16 * | 5.53 | 8.54 * | 21.25 | 9.99 * | 10.77 * | 6.49 | 4.14 | 9.08 * | 4.12 * | |
STD | 2.21 | 0.72 | 0.72 | 2.32 | 1.10 | 1.06 | 0.81 | 0.36 | 0.82 | 0.40 | |
r | 3.58 | 1.09 | 1.78 | 4.29 | 1.98 | 2.19 | 1.31 | 0.91 | 1.84 | 1.82 | |
R | 6.97 | 2.24 | 2.56 | 7.55 | 3.56 | 3.55 | 2.56 | 1.30 | 2.82 | 1.98 | |
N | 16 | 16 | 16 | 13 | 16 | 16 | 14 | 17 | 15 | 16 |
a Mean: mean yield (μg/cig) except TPM (mg/cig) and puff count (pc)
b STD: overall standard deviation
c r: repeatability (μg/cig at 95% confidence interval)
d R: reproducibility (μg/cig at 95% confidence interval)
e N: number of datasets used for r and R determination after removal of outliers and non-quantifiable values
* Values calculated after removal of outlier (s)
Through this study, a robust method CRM Nº 78 (23) and ISO standards ISO 23904 (24) and ISO 23905 (25) were established for the determination of mainstream cigarette smoke phenolics.
The scope of the study included 20 laboratories testing 10 cigarette samples across a range of blends types. The products tested included a range of TPM values between 1 mg and 16 mg (ISO 3308) and 32 mg and 51 mg (ISO 20778) and two smoking machine designs. The analytes tested were from a 4-fold to a 60-fold range in of the analytes of interest. Reproducibility (R) values, expressed as a percentage of mean yield, ranged from 17–150%.
Participating laboratories and product volunteers.
Testing participants | |
---|---|
Altria Client Services | ITC Ltd. |
ARISTA Laboratories | ITG, France |
BAT Souza Cruz SA – Brazil | ITL – Reemtsma Cigarettenfabriken |
British American Tobacco | Japan Tobacco Inc. |
China National Tobacco Corp. Beijing Cigarette Factory | Japan Tobacco International |
CNTC – Zhengzhou Tobacco Research Institute | KT&G Corp. |
CNTC QC | Labstat International Inc. |
Enthalpy Analytical, Inc. | Philip Morris International – Brazil |
Essentra Scientific Services | Philip Morris International – Indonesia |
Global Laboratory Services, Inc. | R.J. Reynolds Tobacco Co. |
Intense smoking regime – Inter-laboratory mean yields, repeatability (r) and reproducibility (R) data.
CM7 | 1R5F | 3R4F | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | ||
---|---|---|---|---|---|---|---|---|---|---|---|
Puff count | Mean |
11.78 | 6.40 | 10.39 | 7.00 | 9.74 | 7.62 | 5.81 | 5.02 | 9.31 | 6.54 |
STD |
0.56 | 0.36 | 0.51 | 0.40 | 0.51 | 0.52 | 2.63 | 1.25 | 2.33 | 0.37 | |
TPM | Mean | 43.36 | 31.83 | 44.12 | 44.11 | 40.16 | 45.09 | 24.62 | 19.43 | 33.86 | 25.79 |
STD | 6.09 | 4.07 | 3.97 | 4.80 | 4.62 | 4.87 | 12.32 | 5.91 | 9.33 | 3.76 | |
Hydroquinone | Mean | 191.17 | 53.41 | 89.62 | 91.44 | 101.85 | 114.04 | 76.44 |
43.56 | 106.50 | 60.19 |
STD | 15.16 | 5.08 | 7.49 | 7.99 | 8.60 | 6.30 | 5.32 | 4.30 | 9.49 | 5.47 | |
r |
27.40 | 11.85 | 11.67 | 18.19 | 15.75 | 18.27 | 9.98 | 9.36 | 15.97 | 17.18 | |
R |
49.02 | 17.74 | 23.43 | 27.67 | 27.88 | 24.05 | 17.37 | 14.67 | 30.16 | 21.70 | |
N |
18 | 17 | 18 | 14 | 18 | 18 | 14 | 18 | 16 | 18 | |
Resorcinol | Mean | 3.77 | 1.07 |
1.87 |
1.35 |
2.55 | 2.77 | 2.21 | 2.07 | 2.70 | 1.46 |
STD | 0.79 | 0.15 | 0.40 | 0.41 | 0.68 | 0.79 | 0.48 | 0.44 | 0.39 | 0.42 | |
r | 0.70 | 0.38 | 0.45 | 0.60 | 0.65 | 0.75 | 0.80 | 0.68 | 0.71 | 0.57 | |
R | 2.31 | 0.55 | 1.18 | 1.27 | 1.99 | 2.32 | 1.52 | 1.39 | 1.26 | 1.27 | |
N | 18 | 14 | 15 | 11 | 17 | 18 | 15 | 17 | 16 | 17 | |
Catechol | Mean | 198.81 | 41.73 | 90.24 | 76.29 | 100.18 | 96.21 | 79.79 |
54.38 | 127.00 |
51.10 |
STD | 15.11 | 3.55 | 6.71 | 6.52 | 7.92 | 9.10 | 6.22 | 4.56 | 6.48 | 5.27 | |
r | 27.35 | 9.81 | 14.58 | 14.03 | 14.46 | 20.19 | 11.53 | 12.81 | 24.78 | 13.13 | |
R | 48.87 | 13.26 | 22.87 | 22.16 | 25.68 | 31.23 | 20.24 | 17.16 | 28.64 | 18.86 | |
N | 18 | 17 | 18 | 14 | 18 | 18 | 14 | 18 | 15 | 18 | |
Phenol | Mean | 43.05 | 8.20 | 13.13 | 36.65 | 16.99 | 19.19 | 12.00 | 6.64 | 19.33 |
6.93 |
STD | 3.59 | 0.91 | 1.05 | 1.20 | 1.46 | 1.59 | 1.33 | 0.63 | 1.35 | 0.57 | |
r | 8.93 | 1.88 | 3.30 | 8.39 | 4.14 | 4.82 | 2.96 | 1.74 | 4.59 | 3.13 | |
R | 12.83 | 3.05 | 4.17 | 8.22 | 5.51 | 6.21 | 4.56 | 2.34 | 5.58 | 3.23 | |
N | 18 | 17 | 18 | 14 | 18 | 18 | 15 | 18 | 15 | 18 | |
Mean | 8.67 | 2.53 | 4.15 | 10.88 | 4.66 | 5.22 | 3.14 |
1.90 | 4.53 |
1.97 | |
STD | 1.14 | 0.28 | 0.50 | 0.99 | 0.60 | 0.60 | 0.38 | 0.22 | 0.41 | 0.28 | |
r | 1.89 | 0.58 | 0.96 | 2.52 | 1.05 | 1.22 | 0.66 | 0.52 | 1.15 | 0.91 | |
R | 3.62 | 0.93 | 1.64 | 3.58 | 1.93 | 2.01 | 1.22 | 0.78 | 1.55 | 1.13 | |
N | 18 | 16 | 18 | 14 | 18 | 18 | 14 | 17 | 15 | 17 | |
Mean | 7.08 | 1.78 | 3.25 | 7.14 | 3.58 | 3.90 | 2.65 | 1.58 | 3.91 | 1.67 | |
STD | 1.07 | 0.22 | 0.45 | 0.74 | 0.51 | 0.37 | 0.43 | 0.22 | 0.37 | 0.35 | |
r | 1.27 | 0.48 | 0.72 | 1.49 | 0.68 | 0.90 | 0.64 | 0.45 | 0.84 | 0.69 | |
R | 3.22 | 0.76 | 1.42 | 2.47 | 1.55 | 1.31 | 1.34 | 0.74 | 1.28 | 1.16 | |
N | 17 | 16 | 17 | 13 | 17 | 16 | 14 | 17 | 16 | 17 | |
Mean | 20.16 |
5.53 | 8.54 |
21.25 | 9.99 |
10.77 |
6.49 | 4.14 | 9.08 |
4.12 |
|
STD | 2.21 | 0.72 | 0.72 | 2.32 | 1.10 | 1.06 | 0.81 | 0.36 | 0.82 | 0.40 | |
r | 3.58 | 1.09 | 1.78 | 4.29 | 1.98 | 2.19 | 1.31 | 0.91 | 1.84 | 1.82 | |
R | 6.97 | 2.24 | 2.56 | 7.55 | 3.56 | 3.55 | 2.56 | 1.30 | 2.82 | 1.98 | |
N | 16 | 16 | 16 | 13 | 16 | 16 | 14 | 17 | 15 | 16 |
Elution program.a
Time (min) | Composition | |
---|---|---|
% A | % B | |
0 | 78 | 22 |
8 | 78 | 22 |
8.5 | 55 | 45 |
21 | 55 | 45 |
22 | 0 | 100 |
28 | 0 | 100 |
(Equilibrate 6 min) |
Non-intense smoking regime – Inter-laboratory mean yields, repeatability (r) and reproducibility (R) data.
CM7 | 1R5F | 3R4F | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | Sample 7 | ||
---|---|---|---|---|---|---|---|---|---|---|---|
Puff count | Mean |
8.45 | 6.90 | 8.28 | 5.66 | 7.88 | 6.91 | 5.19 | 4.54 | 6.82 | 6.16 |
STD |
0.35 | 0.27 | 0.33 | 0.27 | 0.36 | 0.34 | 2.35 | 1.10 | 1.65 | 0.25 | |
TPM | Mean | 16.12 | 1.96 | 9.85 | 13.46 | 8.85 | 10.24 | 3.26 | 1.69 | 10.64 | 1.17 |
STD | 1.07 | 0.32 | 0.78 | 1.78 | 0.75 | 0.84 | 1.71 | 0.52 | 2.90 | 0.31 | |
Hydroquinone | Mean | 91.82 | 8.45 | 32.84 | 42.78 | 36.98 | 46.88 | 20.38 |
9.30 | 46.69 | 8.09 |
STD | 7.47 | 1.33 | 2.78 | 3.85 | 3.43 | 3.60 | 3.26 | 1.19 | 4.08 | 0.96 | |
r |
12.14 | 1.58 | 4.27 | 8.92 | 5.97 | 6.72 | 2.89 | 1.78 | 6.31 | 1.41 | |
R |
23.58 | 3.97 | 8.67 | 13.40 | 10.99 | 11.75 | 9.49 | 3.68 | 12.73 | 2.97 | |
N |
18 | 17 | 18 | 14 | 18 | 18 | 14 | 18 | 16 | 18 | |
Resorcinol | Mean | 1.79 |
0.13 |
0.63 |
0.66 |
0.80 |
0.97 |
0.51 | 0.35 | 1.19 |
0.12 |
STD | 0.30 | 0.04 | 0.15 | 0.21 | 0.16 | 0.18 | 0.09 | 0.05 | 0.21 | 0.03 |
|
r | 0.52 | 0.09 | 0.19 | 0.37 | 0.29 | 0.29 | 0.18 | 0.14 | 0.22 | 0.10 | |
R | 0.95 | 0.14 | 0.46 | 0.67 | 0.51 | 0.58 | 0.30 | 0.17 | 0.63 | 0.13 | |
N | 17 | 13 | 15 | 12 | 16 | 16 | 13 | 15 | 15 | 12 | |
Catechol | Mean | 96.39 | 8.13 | 36.77 | 35.30 | 39.87 | 42.61 | 24.17 | 12.89 | 58.19 | 7.84 |
STD | 4.13 | 0.62 | 1.72 | 1.53 | 2.45 | 2.16 | 2.41 | 0.68 | 3.09 | 0.59 | |
r | 13.39 | 1.60 | 5.02 | 7.32 | 6.84 | 4.91 | 4.77 | 1.98 | 7.58 | 1.88 | |
R | 16.65 | 2.25 | 6.60 | 7.83 | 9.19 | 7.46 | 7.99 | 2.61 | 11.00 | 2.35 | |
N | 18 | 17 | 18 | 14 | 18 | 17 | 15 | 18 | 16 | 18 | |
Phenol | Mean | 27.60 |
0.93 | 7.06 | 19.97 | 9.64 | 12.47 | 4.58 | 1.21 |
13.91 | 0.49 |
STD | 2.94 | 0.19 | 0.80 | 1.49 | 1.28 | 1.15 | 1.11 | 0.25 | 1.42 | 0.11 | |
r | 4.17 | 0.44 | 1.59 | 4.12 | 2.43 | 2.52 | 1.24 | 0.36 | 3.04 | 0.29 | |
R | 9.05 | 0.65 | 2.64 | 5.57 | 4.20 | 3.93 | 3.30 | 0.77 | 4.81 | 0.39 | |
N | 16 | 14 | 18 | 14 | 18 | 18 | 15 | 16 | 16 | 13 | |
Mean | 5.63 | 0.38 | 2.33 | 5.75 | 2.62 | 3.30 | 1.34 | 0.42 |
3.40 | 0.21 | |
STD | 0.68 | 0.08 | 0.27 | 0.65 | 0.37 | 0.35 | 0.26 | 0.10 | 0.43 | 0.07 | |
r | 0.96 | 0.15 | 0.54 | 1.22 | 0.63 | 0.67 | 0.29 | 0.15 | 0.66 | 0.12 | |
R | 2.08 | 0.25 | 0.90 | 2.11 | 1.18 | 1.14 | 0.78 | 0.31 | 1.35 | 0.23 | |
N | 18 | 15 | 18 | 14 | 18 | 18 | 15 | 16 | 16 | 13 | |
Mean | 4.57 | 0.32 | 1.83 | 3.73 | 2.03 | 2.50 | 1.10 | 0.38 | 2.78 | 0.24 | |
STD | 0.67 | 0.10 | 0.18 | 0.45 | 0.33 | 0.29 | 0.22 | 0.07 | 0.28 | 0.12 | |
r | 0.69 | 0.12 | 0.37 | 0.77 | 0.42 | 0.43 | 0.23 | 0.11 | 0.53 | 0.10 | |
R | 1.98 | 0.29 | 0.61 | 1.43 | 0.99 | 0.90 | 0.64 | 0.23 | 0.92 | 0.36 | |
N | 17 | 13 | 17 | 13 | 17 | 17 | 14 | 17 | 16 | 13 | |
Mean | 12.45 | 0.73 | 4.56 | 10.40 | 5.44 | 6.49 | 2.49 | 0.88 | 6.25 | 0.44 | |
STD | 1.24 | 0.14 | 0.51 | 0.87 | 0.71 | 0.60 | 0.50 | 0.13 | 0.73 | 0.13 | |
r | 1.63 | 0.27 | 0.75 | 2.24 | 1.19 | 1.07 | 0.47 | 0.20 | 1.02 | 0.16 | |
R | 3.76 | 0.46 | 1.58 | 3.16 | 2.26 | 1.93 | 1.47 | 0.40 | 2.24 | 0.39 | |
N | 17 | 16 | 17 | 13 | 17 | 17 | 14 | 17 | 16 | 17 |
Study samples.
Sample ID | Blend description | Approximate TPM ISO 3308 regime (mg/cig) |
Approximate TPM ISO 20778 regime (mg/cig) |
---|---|---|---|
CM7 | Virginia | 16.1 | 43.4 |
KR 1R5F | American | 2.0 | 31.8 |
KR 3R4F | American | 9.9 | 44.1 |
Sample 1 | Dark air-cured | 13.5 | 44.1 |
Sample 2 | American | 8.9 | 40.2 |
Sample 3 | American | 10.2 | 45.1 |
Sample 4 | Virginia | 4.0 | 30.3 |
Sample 5 | Virginia | 1.8 | 20.6 |
Sample 6 | Virginia | 11.3 | 36.1 |
Sample 7 | Charcoal filtered | 1.2 | 25.8 |
Fluorescence detector settings.
Time initial | Excitation (nm) | Emission (nm) |
---|---|---|
0.0 | 280 | 310 |
12.4 | 280 | 310 |
12.5 | 274 | 298 |
23.0 | 274 | 298 |
24.0 | 280 | 310 |
28.0 | 280 | 310 |