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

8

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


60 puffs/Collection


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

12

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%



13

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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0

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)

15

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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cambridge filter pad collection efficiency of … · presentation no 46. 2016_tsrc46_sharifi.pdf...

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