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
2
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
3
Preparation for Smoking
4
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
5
6
Non-Cylindrical Mouth End (ME)
7
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
8
Adjusted mouth-end cutting distance from the Standard to
avoid disturbing the wrapper
Puff Volume Determination (mL/puff)
From CRM 65:
9
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
10
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
11
Smoking
12
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
13
Ash build-up smothers coals
14
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
15
Smoke Formaldehyde
16
0
5
10
15
20
25
30
35
A B C D E F
µg/cigarFormaldehyde
n=7, error bars = 1stdev
0
100
200
300
400
500
600
A B C D E F
/cigar
Tar (mg)
Puff Ct
CO (mg)
A
B
C
D
E
F
Lab Comparison – Smoke Formaldehyde
17
0
5
10
15
20
25
30
35
A B C D E F
µg/cigar
Lab 1
Lab 2
Lab 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
18
Butane Gas Contamination Check for VOC
• None Noted
19
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
12
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
20
Reporting Units for Comparison Work
21
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
22

Coresta2017 tayyarah st04

  • 1.
    Challenges and considerationsfor 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
  • 2.
    Topics • Sample Storage& Conditioning • Preparation for smoking • Smoking • Data analysis 2
  • 3.
    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 3
  • 4.
  • 5.
    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 5
  • 6.
  • 7.
    Non-Cylindrical Mouth End(ME) 7 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
  • 8.
    Wrapper fall offduring ME cutting 8 Adjusted mouth-end cutting distance from the Standard to avoid disturbing the wrapper
  • 9.
    Puff Volume Determination(mL/puff) From CRM 65: 9 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
  • 10.
    Choice of CigarHolder • In progress CORESTA technical guides will help 10
  • 11.
    Lab References/Controls • Productyields 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 11
  • 12.
  • 13.
    Lighting Technique High numberof 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 13
  • 14.
  • 15.
    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 15
  • 16.
    Smoke Formaldehyde 16 0 5 10 15 20 25 30 35 A BC D E F µg/cigarFormaldehyde n=7, error bars = 1stdev 0 100 200 300 400 500 600 A B C D E F /cigar Tar (mg) Puff Ct CO (mg) A B C D E F
  • 17.
    Lab Comparison –Smoke Formaldehyde 17 0 5 10 15 20 25 30 35 A B C D E F µg/cigar Lab 1 Lab 2 Lab 3 n=7, error bars = 1stdev
  • 18.
    Will lighting techniqueinfluence analytes? • Additional testing needed for methods validation work • If there is an influence and no standards, there will be bias between labs 18
  • 19.
    Butane Gas ContaminationCheck for VOC • None Noted 19 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 12 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
  • 20.
  • 21.
    Reporting Units forComparison Work 21
  • 22.
    Conclusions • There aremany 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 22