CAMBRIDGE FILTER PAD COLLECTION EFFICIENCY OF … · Presentation no 46. 2016_TSRC46_Sharifi.pdf...
Transcript of CAMBRIDGE FILTER PAD COLLECTION EFFICIENCY OF … · Presentation no 46. 2016_TSRC46_Sharifi.pdf...
Mehran SHARIFI, Peter JOZA, Romulo LODEVICO, Bill RICKERT
CAMBRIDGE FILTER PAD COLLECTION EFFICIENCY OF MENTHOL FROM E-CIGARETTE AEROSOLS – AN
INVESTIGATIVE STUDY
70th TOBACCO SCIENCE RESEARCH CONFERENCESeptember 18-21, 2016
Palm Beach Gardens, Florida, USA
LABSTAT INTERNATIONAL ULC.262 Manitou Drive
Kitchener, Ontario, Canada N2C 1L3Phone: (519) 748-5409 Fax: (519) 748-1654
www.labstat.com
Presentation no 46
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To evaluate the performance efficiency of Cambridge pad filter for collecting menthol in e-cigarette aerosols.
Objective
To identify the factors affecting both CFP collection efficiency and analyte transfer to aerosol.
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Typical collection methodologies used for trapping constituents in tobacco mainstream smoke are based on three approaches:
Adequacy of Current Methodologies for Exploration of E-cigarette Emissions?
Cambridge Filter Pad (CFP)
Direct Solvent Collection (Impinger)
Combined Filter Pad + Impinger
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Plan of the Presentation
I Cambridge Filter Pad Collection Efficiency: Cigarette Smoke vs E-Cigarette Aerosol
Suitability for collecting Menthol (breakthrough?) Suitability for other analytes in e-aerosols (i.e. humectants or degradation compounds Impact of puffing intensity on breakthrough rate
II Factors Affecting CFP Collection Efficiency and Analyte Transfer into Aerosol
PG/Glycerol composition ratio in e-liquid Water content in e-liquid
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Glycidol
Prop
ylen
e G
lyco
l
Menthol
Anethol(ISTD)
Nicotine
Inte
nsity
(mVo
lts)
Minutes
Ethy
lene
Gly
col
Glycerol
Menthol, Nicotine and Humectants
5
E-Cigarette Linear Smoking
Machine
Cambridge Filter Pad+
Impinger(Isopropanol)
Impinger Content
Extract CFP with Isopropanol
GC-FID Analysis
DB-WAX 15m, 0.53mm, 1µm
Injector: 220°C
Detector: 260°C
Temp. Program:
120°C for 2 min,15°C/min to 180°C,180°C for 4 min
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Investigative Study 1
• CFP efficiency for collecting menthol from aerosol?
• Puffing regimen (“aerosol load”) impact on CFP collection efficiency?
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Investigative Study 1 - Experimental
Test Products Puffing Regime(Volume/Duration/Frequency)
Puff Counts (/Collection)
ACM(mg/Collection)
Menthol-containing Cigalike 80/3/3055/3/3035/2/60
1006075
20814063
TPM(mg/Collection)
Menthol Tobacco Cigarette 55/2/30 100% Blocked35/2/60
30±137±0.5
13595
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• Less than 1% menthol breakthrough in cigarette mainstream smoke.
• Menthol in e-aerosols is not completely trapped on CFP.
• Menthol breakthrough increases directly with Accumulated Mass (ACM).
Analytical Results - Menthol Breakthrough
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0%
10%
20%
30%
40%
50%
60%
70%
80%
90%
100%
35/2/60 55/3/30 80/3/30 ISO Intense
4% 6%9%
< 1% < 1%
RELA
TIVE
DIS
TRIB
UTI
ON
PUFFING CONDITIONS
Pad Menthol Impinger Menthol
E-Cigarette Aerosol Cigarette Smoke • Less than 1% menthol breakthrough in cigarette mainstream smoke.
• Less than 1% menthol breakthrough in cigarette mainstream smoke.
• Menthol in e-aerosols is not completely trapped on CFP.
R² = 0.9819
0
2
4
6
8
10
0 100 200 300
Men
thol
Bre
akth
roug
h(%
of T
otal
)
Accumulated Mass (mg/collection)
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Analytical Results - Breakthrough Composition
Glycidol
Ethylene Glycol Menthol
NicotinePropylene Glycol
𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 𝐶𝐶𝐵𝐵𝐶𝐶𝐶𝐶𝐵𝐵𝐶𝐶𝐶𝐶𝐵𝐵𝐶𝐶𝐵𝐵𝐶𝐶 % =)𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 Each Analyte (%
𝑇𝑇𝐵𝐵𝐵𝐵𝐵𝐵𝑇𝑇 𝐵𝐵𝑜𝑜 𝐴𝐴𝑇𝑇𝑇𝑇 𝐴𝐴𝐶𝐶𝐵𝐵𝑇𝑇𝐴𝐴𝐵𝐵𝐵𝐵𝐶𝐶 𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 (%)× 100
Filter Pad Efficiency
Analyte Contributionto
Total Analytes Breakthrough
Glycerol None
Propylene Gly. 2% of Total
Nicotine 1% of Total
Menthol × 16% of Total
Ethylene Gly. × 40 % of Total
Glycidol × 41 % of Total
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Analytical Results - Glycidol / Ethylene glycol / Menthol
Under 80/3/30 puffing regimen:
• Menthol exhibited ca. 10% breakthrough.
• Glycidol and Ethylene glycol exhibited approximately 24% breakthrough.
𝐴𝐴𝐶𝐶𝐵𝐵𝑇𝑇𝐴𝐴𝐵𝐵𝐵𝐵 𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵𝐵 % =][𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼 𝑐𝑐𝐵𝐵𝐶𝐶𝐵𝐵𝐵𝐵𝐶𝐶𝐵𝐵
]𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼 𝑐𝑐𝐵𝐵𝐶𝐶𝐵𝐵𝐵𝐵𝐶𝐶𝐵𝐵 + [𝐼𝐼𝐴𝐴𝑃𝑃 𝑐𝑐𝐵𝐵𝐶𝐶𝐵𝐵𝐵𝐵𝐶𝐶𝐵𝐵× 100
24.2 % 23.9 %
9.3%
0.0
5.0
10.0
15.0
20.0
25.0
30.0
Glycidol Ethylene Glycol Menthol
Brea
kthr
ough
(% )
Ethylene Glycol
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Summary - CFP Suitability
AnalyteCigarette Smoke
35/2/6055/2/30 100% Blocked
E-cig Aerosol35/2/60
75 puffs/Collection
E-cig Aerosol55/3/30
60 puffs/Collection
E-cig Aerosol80/3/30
100 puffs/Collection
Breakthrough (%)Menthol < 1 4 6 9.3
Glycidol ND - - 24.2
Ethylene glycol ND - - 23.9
Propylene glycol ND - - 2
Nicotine < 1 - - < 1
Glycerol ND - - 0
Diethylene glycol ND ND ND ND
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Investigative Study 2
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PG/GLY composition of e-liquid
Water content of e-liquid
What are the factors affecting CFP “Collection Efficiency” in e-aerosols? How about “analyte transfer”?
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PG:Gly (10:90) - 10% PG:Gly (50:50) - 10% PG:Gly (90:10) - 10%
PG:Gly (10:90) - 5% PG:Gly (50:50) - 5% PG:Gly (90:10) - 5%
PG:Gly (10:90) - 1% PG:Gly (50:50) - 1% PG:Gly (90:10) - 1%
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Test Design - E-Liquid CompositionW
ater
Con
tent
(%)
Propylene Glycol : Glycerol Ratio
Each e-liquid matrix was spiked with known amounts of target analytes at two different levels.
The amounts of analytes added to the matrix was calculated such that a 2 % breakthrough into the impinger would be quantifiable.
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Experimental - Sample Generation
Puffing Parameters/Settings Purpose
E-cigarette Settings (Clearomizer system)
Voltage 5.0VResistivity 1.7ΩAir intake orifice Φ1.8mm
High-energy atomizer device settings were chosen to maximize the aerosol release.
Puffing Conditions 80 ± 0.5 mL puff volume, 3.0 ± 0.03 sec duration,30 ± 0.5 sec intervalSquare wave puff profile75 puffs per observation
Extreme puffing conditions were chosen to maximize the likelihood of breakthrough
Device Performance Control
Pad/holder weight prior/after puffing
Tank/atomizer weight prior/after puffing
To calculate the weight of collected Particulate Phase (Accumulated Mass)
To calculate e-liquid consumption per collection (Device Mass Loss)
Analysis Extraction/analysis of analyte contents in CFP and Impinger, separately.
Evaluation of analyte breakthrough
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200
400
600
800
1000
1200
1400
1600
0 500 1000 1500 2000
Accu
mul
ated
Mas
s (m
g/co
llect
ion)
E-liquid Consumption (mg/collection)
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Analytical Results - E-liquid Composition on PG and Gly Transfer
R2 = 0.653
XXX
Glycerol Aerosol Propylene Glycol Aerosol
PG:G
ly(9
0:10
)
Low 10%
High 10%
Low 5%
High 5%
Low 1%
High 1%
PG:G
ly(5
0:50
) Low 10%
High 10%
Blank 5%
Blank 5%
High 1%
PG:G
ly(1
0:90
)
Low 10%
High 10%
Low 5%
High 5%
Low 1%
High 1%
E-liquid Composition
AnalyteContent
WaterContent
Relative percentage in Aerosol (%)
X
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Analytical Results -Factors Affecting Analyte “Transfer” to Aerosol?
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
Glycidol Propyleneglycol
Ethyleneglycol
Menthol Nicotine DiethyleneGlycol
Triacetin Glycerol
(Log
of A
vera
ge Y
ield
s)
PG:Gly (10:90) PG:Gly (50:50) PG:Gly (90:10) 2016
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E-liquid Water Content: 1% 5% 10% 17
Factors Affecting Analyte “Transfer” to Aerosol?Water Content in E-Liquid
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5Glycidol
Propylene glycol
Ethylene Glycol
Menthol
Nicotine
Diethylene Glycol
Triacetin
Glycerol
Aerosol Yields (Logarithmic Scale)
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5Glycidol
Propylene glycol
Ethylene Glycol
Menthol
Nicotine
Diethylene Glycol
Triacetin
Glycerol
Aerosol Yields (Logarithmic Scale)
PG:Gly (10:90) PG:Gly (90:10)
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Analytical Results – Analytes Breakthroughs
E-Liquid Water
Content
E-LiquidGly / PG
Composition
Propylene Glycol(%)
Glycidol(%)
1%
10 / 90
0.19 4.85% 0.24 3.610% 0.22 7.2
1%
90 / 10
0.65 15.7
5% 0.66 11.3
10% 0.62 17.3
Breakthrough was only observed for Glycidol and Propylene glycol.
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Analytical Results - Glycidol Breakthrough
10% 7%8% 8%
4% 4%5%
0
20
40
60
80
100
120
140
160
Glyc
idol
(µg/
g Ac
cum
ulat
ed M
ass)
Impinger Content CFP Content
Water Content 1% 5% 10% - 10% 1% 5% 10% 5%
PG:Gly Composition 10:90 50:50 90:10 50:50
E-liq. Analyte Levels High Content Blank
Lower glycidol breakthrough observed for formulations containing 90% PG.
H2O Content in E-liquid does not affect the breakthrough rate.
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Analytical Results - Glycidol Breakthrough
10% 7%8% 8%
4% 4%5%
21% 16%
26%
40%
6% 10%
0
20
40
60
80
100
120
140
160
Glyc
idol
(µg/
g Ac
cum
ulat
ed M
ass)
Impinger Content CFP Content
Water Content 1% 5% 10% - 10% 1% 5% 10% 1% 5% 10% 10% 1% - 10% 5%
PG:Gly Composition 10:90 50:50 90:10 10:90 50:50 90:10 50:50
E-liq. Analyte Levels High Content Low Content Blank
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Summary (2nd investigative study)
• The results of the 2nd study did not confirm our previous observations with respect to menthol breakthrough (simply not observed)!?
This may be attributed to:
Differences between e-cigarette devices Power, resistance, wick material, etc… Refillable e-liquid tank system vs. Cigalike e-devices
Differences in e-liquid compositions Contribution of other compounds (i.e. flavoring agents) in the commercial
Cigalike products that would favor menthol breakthrough.
• A combination of high water/glycerol contents in e-liquid can increase (ca. 10-30 %) the transfer rates of Diethylene glycol, menthol, nicotine and ethylene glycol.
• Glycidol exhibited a significant amount of breakthrough under 80/3/30 puffing regimen. It was demonstrated that glycidol breakthrough increases with glycerol content in e-liquid/aerosol.
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Conclusion
It is recommended that an impinger be included when determining glycidol, ethylene glycol or menthol contents of e-aerosols regardless of the puffing regimen, e-liquid composition or vaporizer type (i.e. Cigalike or refillable tank).
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Acknowledgment
Thank you for Your Attention!
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