Comparison of select analytes in tobacco and smoke for cigar products across a range of design features

TAYYARAH R.; ZHU J.; BROOKS C.; STEVENS R.

Rana.Tayyarah@itgbrands.com CORESTA 2017 ST03

Objectives

• Evaluation of Cigar products with a range of design features

• Assessment of analytical variability across labs

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Study Design

• 6 Cigar products of varying design and yield • Lot matched samples tested at 3 laboratories • Select tobacco and smoke analytes typical of cigarette

testing • TNCO according to CORESTA CRM 46/64/65 • Smoking for other analytes using applicable Cigar CRM

parameters • Other methodology not specified

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Study Sample Set – A range of designs

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A B

C

D E F

Tobacco Measurements

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Cigar Tobacco Content Cigar A B C D E F

Nicotine µg/g 11065 22419 8336 9742 23666 29138

Ammonia µg/g 2771 4769 2116 1616 6990 8593

Cadmium ng/g 1078 1164 1173 1326 527 722

Arsenic ng/g 98.9 146 2342 2080 111 133

NNN ng/g 5326 3012 10016 1850 2186 2050

NNK ng/g 4682 661 4388 445 687 164

BaP ng/g 4.33 4.63 4.57 4.14 3.86 1.85

Formaldehyde µg/g 1.22 0.510 0.715 3.33 1.19 1.39

Acetaldehyde µg/g 1.17 0.213 0.967 0.292 0.650 1.28

Crotonaldehyde µg/g <LOD <LOD <LOD <LOD <LOD <LOD

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Averaged data shown are from a single laboratory n=7; aliquots taken before grinding Typical analytes for cigarette and/or smokeless tobacco products

Cigar Tobacco Content Cigar A B C D E F Highest %RSD

for Set Nicotine µg/g 11065 22419 8336 9742 23666 29138 4%

Ammonia µg/g 2771 4769 2116 1616 6990 8593 2% Cadmium ng/g 1078 1164 1173 1326 527 722 11%

Arsenic ng/g 98.9 146 2342 2080 111 133 24% NNN ng/g 5326 3012 10016 1850 2186 2050 7% NNK ng/g 4682 661 4388 445 687 164 11% BaP ng/g 4.33 4.63 4.57 4.14 3.86 1.85 8%

Formaldehyde µg/g 1.22 0.510 0.715 3.33 1.19 1.39 15% Acetaldehyde µg/g 1.17 0.213 0.967 0.292 0.650 1.28 19%

Crotonaldehyde µg/g <LOD <LOD <LOD <LOD <LOD <LOD --

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Averaged data shown are from a single laboratory n=7; aliquots taken before grinding Typical analytes for cigarette and/or smokeless tobacco products

Lab Comparison – Tobacco Nicotine

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0

5000

10000

15000

20000

25000

30000

35000

40000

A B C D E F

µg/g

Lab 1Lab 2Lab 3

n=7 Error bars = 3*standard deviation

Physical Parameters

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Cigar Physicals – Range & Variability

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Cigar A B C D E F High %RSD of Set

Conditioned Cigar Weight g/cig 1.36 2.69 2.97 3.91 13.87 18.05 9%

Conditioned Tobacco Weight g/cig 1.0 2.2 2.6 2.2 13.5 17.6 11%*

Length mm 98.3 98.5 113.7 121.4 127.0 151.6 1.2%

Circumference mm 24.2 31.2 33.4 35.6 62.2 65.9 2.2%

Pressure Drop mmH2O 260.7 104.7 127.3 96.3 37.4 37.9 43%

Averaged data shown are from a single laboratory n=20 *Conditioned weight CM8 cigarette typically <1% RSD

Lab Comparison – Pressure Drop

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-50

0

50

100

150

200

250

300

350

A B C D E F

mm

H2O

/cig

ar

Lab 1Lab 2Lab 3

n=20 Error bars, if shown, = 3 * standard deviation

TNCO Measurements

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CRM 64/65 Highlights • Smoke 1 or 2 cigars based on diameter per trap*

• Puffing Volume – varies with Cigar Diameter – 20mL ≤12.0 mm diameter – 0.139*diameter2 if >12.0 mm diameter

• Puff Frequency, 1 puff every 40s

• Puff duration, 1.5s

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*Notes: current for current CRM 1 replicate = 8 cigars, in this case 1 replicate = 1 individual measurement (i.e. 1 pad) ≤12.0 rather than <12.0 is a planned CRM update

Cigar TNCO – Range & Variability

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Cigar A B C D E F High %RSD of Set

Puff ct /cigar 21 54 45 37 92 201 29%

CO mg/cigar 28 65 69 58 360 553 64%

Nicotine mg/cigar 0.95 2.3 1.5 1.1 5.6 22 61%

Tar mg/cigar 22 37 49 31 92 138 51%

Averaged data shown are from a single laboratory n=20

Product Comparison – Tar Yields

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• Products are not as distinguished as expected by the range of design features

mg/

ciga

r

Sample data shown are from a single laboratory n=20

Product Comparison – Smoke Water

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Sample

Note: Highest yielding replicate for Sample F ~600mg/cigar (TPM 750mg) data shown are from a single laboratory n=20

Smoke Constituents

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Smoke Analytes – Range across Products

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Average Yield Sample Rep %RSD Low Avg Yield High Avg Yield Highest %RSD

Ammonia µg/cigar 28 5987 121% Formaldehyde µg/cigar 8 15 36% Acetaldehyde µg/cigar 700 5011 41%

Acrolein µg/cigar 11 99 35% Crotonaldehyde µg/cigar 7 77 39% Benzo(a)pyrene ng/cigar 11 155 58%

1,3-butadiene µg/cigar 56 974 43% Isoprene µg/cigar 527 11006 35%

Acrylonitrile µg/cigar 12 473 54% Benzene µg/cigar 58 1634 48% Toluene µg/cigar 84 3705 40%

1-aminonaphthalene ng/cigar 53 518 69% 2-aminonaphthalene ng/cigar 35 271 65%

4-aminobiphenyl ng/cigar 4 50 65% NNN ng/cigar 224 2364 79% NNK ng/cigar 135 689 71%

n=7, single lab values

Smoke Analytes – Product Comparison

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Cigar A B C D E F

Ammonia µg/cig 28 60 107 104 1467 5987

Formaldehyde µg/cig 11 8 11 15 8 9

Acetaldehyde µg/cig 700 955 1721 1769 4669 5011

Acrolein µg/cig 27 11 26 33 63 99

Crotonaldehyde µg/cig 6 9 42 38 61 77

Averaged data shown are from a single laboratory n=7 Typical analytes for cigarette products

Smoke Formaldehyde – Lab Trending

20

05

10152025

A B C D E F

µg/c

igar

n=7

05

10152025

A B C D E F

µg/c

igar

Lab Comparison – Smoke Formaldehyde

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-5

0

5

10

15

20

25

30

35

40

45

A B C D E F

µg/c

igar

Lab 1Lab 2Lab 3

n=7 Error bars = 3* standard deviation

Possible analytical bias with formaldehyde

Smoke Analytes – Product Comparison

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Cigar A B C D E F 1,3-butadiene µg/cig 56 185 235 116 974 974 Isoprene µg/cig 527 2019 1897 1001 8714 11006 Acrylonitrile µg/cig 12 55 72 30 302 473 Benzene µg/cig 58 248 280 152 1313 1634 Toluene µg/cig 84 391 407 230 2700 3705 Carbon Monoxide mg/cig 28 65 69 58 360 553

Averaged data shown are from a single laboratory n=7 Typical analytes for cigarette products

Smoke Analytes – Product Comparison

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Cigar A B C D E F Benzo(a)pyrene ng/cig 11 23 74 32 97 155

1-aminonaphthalene ng/cig 53 90 137 55 424 518

2-aminonaphthalene ng/cig 35 48 78 35 221 270

4-aminobiphenyl ng/cig 4 9 15 5 41 50

NNN ng/cig 350 240 838 224 1303 2364

NNK ng/cig 433 135 689 166 421 380

Averaged data shown are from a single laboratory n=7 Typical analytes for cigarette products

Conclusions

• Cigars with broad design features also have widely varied analyte levels and smoking characteristics

• Variability for physical characteristics are much higher than for cigarette products

• Variability is high enough that it may be difficult to distinguish some products based on analytical data

• For the lab comparison, results appear generally consistent between the labs in the study particularly for Samples A-D

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