Challenges and considerations for methods development and testing of cigar products for smoke constituents beyond TNCO TAYYARAH R.; STEVENS R.; ZHU J.; BROOKS C.;

Rana.Tayyarah@itgbrands.com CORESTA 2017 ST04

Topics

• Sample Storage & Conditioning • Preparation for smoking • Smoking • Data analysis

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Sample Storage & Conditioning

• Cross Contamination from highly flavored products – Attempt to obtain or build small one-way airflow chambers

• Conditioning requirements are straightforward but vary

• Flavored products may not reach equilibrium adding variability due to judgment decision-making

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Preparation for Smoking

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Preparation for Smoking

• Non-symetrical mouth-ends cause judgment with cutting • Diameter determination for non-cylindrical products • No standards for mouth-end cutting • Wrapper fall off

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Non-Cylindrical Mouth End (ME)

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Puff Ct TPM Tar Nicotine CO Water /cigar mg/cig mg/cig mg/cig mg/cig mg/cig

Tipped Avg 37.4 41.6 39.2 1.5 57.4 1.0

%RSD 13 23 22 30 14 106

No-Tip Avg 32.7 30.4 29.0 1.0 46.4 0.4

%RSD 15 36 36 43 28 199

n=7

Wrapper fall off during ME cutting

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Adjusted mouth-end cutting distance from the Standard to avoid disturbing the wrapper

Puff Volume Determination (mL/puff)

From CRM 65:

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Determination* Sample 1 Sample 2

Lab 1 63 mL 75 mL Lab 2 56 65 Lab 3 49 63

*As determined by different testing labs testing the same product batches

Possible Causes for Differences: • Measurement error • Product variability • Technique used • Calculation error

Choice of Cigar Holder

• In progress CORESTA technical guides will help

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Lab References/Controls

• Product yields and designs are highly varied • There are no standard references or controls Possible Current Options • Spiking of matrix with analytes to determine recoveries • Set of references • Cigarette references

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Smoking

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Lighting Technique High number of relights, non-symetrical burn patterns, need for non-standard lighting

• CORESTA Project 148 is exploring alternative lighting techniques • Recent release of larger electric lighter elements

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Ash build-up smothers coals

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Long Smoke Times - Volatiles

• Puff counts may be >200 • Impinger size and volume • Impinger chilling • Derivitization times

– Too long – As a variable between products

• Overload

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Smoke Formaldehyde

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0

5

10

15

20

25

30

35

A B C D E F

µg/c

igar

For

mal

dehy

de

n=7, error bars = 1stdev

0100200300400500600

A B C D E F

/cig

ar Tar (mg)

Puff CtCO (mg)

A B C

D E F

Lab Comparison – Smoke Formaldehyde

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0

5

10

15

20

25

30

35

A B C D E F

µg/c

igar

Lab 1Lab 2Lab 3

n=7, error bars = 1stdev

Will lighting technique influence analytes?

• Additional testing needed for methods validation work • If there is an influence and no standards, there will be

bias between labs

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Butane Gas Contamination Check for VOC • None Noted

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Note: Butane Lighter – BIC USA Inc, USA –Lot number 7033060006

Note: Procedure – 1 mL MeOH in 2 mL amber GC vial, then 1 mL butane gas was added with 1 mL Luer Lock syringe and vortex mixed prior to analysis. (n=3)

4x10

0

0

0

0

1

1

1

1

1

2

2

2

2

2

3

3

+ TIC SIM VO0004.d

12 23 34 45 56

Counts vs. Acquisition Time (min)

4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21

4x10

0.

0.

0.

0.

1

1.

1.

1.

1.

2

2.

2.

+ TIC SIM VO0011.d

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Counts vs. Acquisition Time (min)

3.4 3.6 3.8 4 4.2 4.4 4.6 4.8 5 5.2 5.4 5.6 5.8 6 6.2 6.4 6.6 6.8

Data Analysis

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Reporting Units for Comparison Work

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Conclusions • There are many basic considerations for testing cigar smoking

– Smoking difficulties especially with limited smoking experience – Product variety & variability – Data analysis for analytical comparison

• There are several unique challenges for methods development

beyond TNCO – Long and/or varied smoking times – Lighting techniques – Lack of controls/reference products – Possible overload of analyte traps

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