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GC-MS analysis of e-liquids taken from e-cigarettes and e-liquids
(e-juice) before use in e-cigarettes
John H. Lauterbach, Ph.D., DABT Lauterbach & Associates, LLC, Macon, GA 31210-4708 USA
Deborah A. Grimm, Ph.D. Coordinated Instrumentation Facility
Tulane University, New Orleans, LA 70118-5698 USA
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Objectives for this presentation • Identify major and minor species in e-liquids
using traditional GC-MS analytical techniques – Main aerosol-forming species (PG, VG) – Flavorful components – Unexpected components
• Determine if published ingredient information was consistent with analytical findings
• Attempt to identify compounds present that might account for the cytotoxicity reported in some e-liquids (Bahl et al., Reproductive Toxicology 2012 34:529-37)
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Analytical approach • Capillary column gas chromatography – mass
spectrometry (GC-MS) has been main tool for analyses of flavors for more than three decades – Ability to separate and identify volatiles and semi-
volatile components of complex mixtures – Long history of use in tobacco industry for analyses
of flavor concentrates, finished flavors, and flavors applied to tobacco products
– Tobacco flavors and flavor concentrates often formulated in propylene glycol (PG)
• These factors make GC-MS the ideal tool for the analyses of e-liquids and their components
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Peppermint flavor 1.2% Nicotine
DB-5 MS column Lab 1
Glycerol
Nicotine
Triacetin
Monoacetin
Caryophyllene
Diacetin
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Example chromatogram 1a
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Example chromatogram 1b Peppermint flavor – TMS
1.2% Nicotine DB-5 MS column
Lab 1 Glycerol
Nicotine
PG
Menthol Carvone
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Example chromatogram 1c Peppermint flavor
1.2% Nicotine SolGel-Wax column
Lab 2
Glycerol
Nicotine
PG Menthol
Monoacetin
Triacetin Diacetin
Carvone
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Peppermint e-liquid
Vendor’s web page
Compound Amount
Propylene glycol Very Large
Malic acid Medium
Vanillin Medium
Acetyl pyrazine Small
Menthol Small
Ethyl acetate Small
Aliphatic acid Very small
Common flavors Very small
Found by analysis
Compound Relative amount
Propylene glycol Very large
Glycerol Large
Monoacetins Large
Diacetins Medium
Triacetin Medium
Menthol Small
Menthone Small
Carvone Small
Pulegone Very small
Anethol Very small
Caryophyllene Very small
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Example chromatogram 2a
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Chocolate flavor 1.2% Nicotine
DB-5 MS column Lab 1
Glycerol
Nicotine
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Example chromatogram 2b
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Chocolate flavor – TMS 1.2% Nicotine
DB-5 MS column Lab 1
Glycerol
Nicotine
Hexitol
PG
Di-PG
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Example chromatogram 2c
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Chocolate flavor 1.2% Nicotine
DB-Wax column Lab 2
ISTD
Chocolate flavor 1.2% Nicotine
SolGel-Wax column Lab 2
Glycerol
Nicotine
PG
Di-PG
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Chocolate e-liquid
Vendor’s web page
Compound Amount
Propylene glycol Very Large
Vanilla extract Large
Terpene alcohol Medium
Acetyl pyrazine Small
Alkyl pyrazine Small
C-5 aliphatic acid Small
Common flavors Small
Found by analysis
Compound Relative amount
Propylene glycol Very large
Glycerol Medium
C-6 sugar alcohol Very small
Dipropylene glycol Very small
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Example chromatogram 3
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Tobacco flavor – PG Free 1.8% Nicotine
SolGel-Wax column Lab 2
Glycerol
Nicotine
Syringol
Vanillin
EtVanillin
EtMaltol
Maltol Cyclotene
PG
Menthol
Acetic acid
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Lagniappe • Most information reported to date on the
mainstream e-cigarette aerosol (MECA) has focused on nicotine content and/or known smoke toxicants
• However, the same techniques that are used for analyses of e-liquids should be useful for analyses of major components of MECA – Collect MECA on Cambridge pad – Health Canada Intensive smoking – 100 puffs (≈ 90 mg) – Extract pad with 2-propanol containing
heptadecane as the internal standard (ISTD)
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Example chromatogram 4
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Chocolate flavor MECA 1.2% Nicotine
SolGel-Wax column Lab 2
Glycerol
Nicotine
ISTD
PG
Di-PG C-14 HC
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Example chromatogram 5
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Tobacco flavor – MECA 1.8% Nicotine
SolGel-Wax column Lab 2
Glycerol
ISTD
Nicotine
? EtMaltol
Syringol
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Concluding remarks • Traditional GC-MS techniques for analyses of
flavors and smoke can be applied to e-liquids and mainstream e-cigarette aerosols (MECA)
• There were differences in e-liquid composition between what was expected and what was found – Are users getting the hedonic properties expected
by the manufacturers of the e-liquids? – Do e-liquid vendors have accurate information on
the composition of the products they are selling? – However, nothing to support report of cytotoxicity
• Is there sufficient flavor transfer for superior consumer satisfaction?
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Acknowledgement
• Some of the GC-MS analyses reported in this presentation were performed by Dr. Andrae Spencer of Global Laboratory Services of Wilson, NC. The author would like to thank Dr. Spencer very much for his excellent scientific work on the GC-MS analyses.
• The lead author of this presentation and Lauterbach & Associates, LLC, are totally responsible for the content of this presentation.
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