tsrc 2015_45 tayyarah
TRANSCRIPT
ABBREVIATED METHOD FOR TNCO ANALYSIS - MODIFIED ISO SMOKING
Rana Tayyarah TSRC 2015 # 45 Contact: [email protected]
Objective and Success Criteria
Objective Develop a method for a 2 day reporting of TNCO
Success criteria
– 2 day reporting – %RSD no more than 2 x ISO – Applicable to a range of conventional cigarette designs – Applicable to ISO smoking parameters – Applicable to a high volume sample set – Applicable to a comparative analysis study
2
Variables Considered
• Conditioning time • Number of Cigarettes • Loose versus packed cigarettes • Standard butt length versus fixed number of puffs
3
Sample Types
• Typical American blend cigarette designs • Menthol and Non-Menthol
Range ISO ‘Tar’ (mg/cig) 3 – 17 Length (mm) 80 – 100 Filter Ventilation (%) 0 – 60
4
Method Establishment - Design
• Launch a separate Logistics Project
• Evaluate major variables with a small set of samples
• Robustness for ‘No Conditioning’
• Method Verification - Baseline Data collection over time
5
Logistics Project
• Collection and logging simultaneous – for a preview of the samples
• Automated Batch-building • Custom Data Review Report • Automated Reported
• Isolated workflows in the lab
• No Repeat analysis window, but loop back cycle
established
6
Method Establishment • Conditioning time (0, 24 hours)
• Number of Cigarettes (1-5)
• Loose versus packed cigarettes
• Fixed butt length versus fixed number of puffs
7
No Conditioning vs ISO
0.00
1.00
2.00
3.00
4.00
5.00
NC, 1 NC, 2 NC, 3 ISO
mg/
cig
'Tar'
NC – No conditioning, no equilibrium weight, smoked day of making, 3 cigs/pad, ISO butt length
0.00
0.10
0.20
0.30
0.40
NC, 1 NC, 2 NC, 3 ISOm
g/ci
g
Nicotine
8
Packed vs Loose – No Conditioning
n ‘Tar’ (mg/cig)
Nicotine (mg/cig)
CO (mg/cig)
Packed 91 13.95 ± 0.68 1.00 ± 0.05 15.98 ± 0.88
Loose 96 13.79 ± 0.65 1.00 ± 0.05 15.68 ± 0.91
All Data* 385 13.90 ± 0.68 1.02 ± 0.05 15.92 ± 0.88
ISO Smoking 248 13.92 ± 0.93 1.04 ± 0.06 16.12 ± 1.04
% Difference 0.1% 2.3% 1.3%
*4 cigs/pad, loose or packed cigarettes, Smoked the same day as making with no equilibrium weights using ISO parameters, ISO butt length 9
6-Puff Variability Comparisons – MS Nicotine
Sample (ISO ‘Tar’) ISO 6 Puff Modified ISO
A – 3 mg 9% 18%, 9%, 5% B – 7 mg 8% 7% C – 14 mg 7% 6% D – 17 mg 7% 6% CM6 4% 4%
Success criteria - %RSD no more than 2x ISO value
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Method Establishment - Results • Conditioning time (0, 24 hours)
– Results were similar, 0 was chosen for baseline study
• Number of Cigarettes (1-5) – Result were similar, 3 cigarettes were chosen for baseline
• Loose versus packed cigarettes
– Result were similar, packed was chosen for baseline study
• Fixed butt length versus fixed number of puffs – Both met criteria, fixed butt length was chosen for baseline study
11
No Conditioning Questions
• Cigarette Equilibration (Age)
• Seasonal Impact
• Dry/Moist Cigarettes
12
Cigarette Equilibration (Short-term Aging)
0
2
4
6
8
10
12
Day 0/1 Day 7 Day 14
‘Tar
’ (m
g/ci
g)
Cigarette Age when Smoked
No Conditioning
24 Hour Conditioning
n=12 13
Impact of Varied Conditioning %RH
3R4F cigarettes conditioned for 2 weeks at target %RH Conditioning temperature = 22◦C Smoking Conditions = 60% RH, 22◦C n=5
456789
1011
0% 20% 40% 60% 80% 100%
Yiel
d (m
g/ci
g)
ISO-3s'Tar'ISO+3s
14
Impact of Varied Conditioning %RH
3R4F cigarettes conditioned for 2 weeks at target %RH Conditioning temperature = 22◦C Smoking Conditions = 60% RH, 22◦C n=5
0.4
0.5
0.6
0.7
0.8
0.9
0% 20% 40% 60% 80% 100%
Yiel
d (m
g/ci
g)
ISO-3sNicotineISO+3s
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Method Verification
• Full ‘tar’ range for samples • Dry season and humid season* • At least 100 data points per sample over time
(*for North Carolina) 16
Verification – Exemplary ‘Tar’ Data
02468
101214161820
E F G H I J K L M
Yiel
d (m
g/ci
g)
ISONew Method
n=40-120 17
Verification – Exemplary Nicotine Data
0
0.2
0.4
0.6
0.8
1
1.2
1.4
E F G H I J K L M
Yiel
d (m
g/ci
g)
ISONew Method
n=40-120 18
Verification – Exemplary Carbon Monoxide Data
02468
101214161820
E F G H I J K L M
Yiel
d (m
g/ci
g)
ISONew Method
n=40-120 19
Conclusions • A 2 day TNCO method was established with no cigarette conditioning, no
equilibrium test, 3cigs/pad, loose or packed cigarettes, fixed butt length or fixed puff number
• The Modified Method meets the technical success criteria – Two day reportable, <2x ISO-variability, compatible with high volume submission
• Streamlined Laboratory workflows are key to meeting reporting objectives
• Yield results similar to ISO for standard butt length version
• Fixed puff testing would require control chart establishment for monitors
• Scope not extended to lab to lab comparisons, long-term consistency, or
alternate regimes
20
Acknowledgements
• Sample Control, Routine Testing Services • Brenda Duncan • Francine Hancock • Olabisi Johnson • Michelle Long • Adrian Watson
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