On-line real-time analysis of e-cigarette vapors and heat-not-burn tobacco … · 2018-02-16 · R. Zimmermann et al. TSCR Conference, Naples, Florida/USA, September 20th- 23rd 2015

R. Zimmermann et al. TSCR Conference, Naples, Florida/USA, September 20th- 23rd 2015

On-line real-time analysis of e-cigarette vapors and heat-not-burn tobacco products by photo-

ionization mass spectrometryR.Zimmermann1, S.Ehlert1,2, T.Streibel1, J.M. Wolter1, J. Heide1, A.Walte2

1 University of Rostock, Chair of Analytical Chemistry, Inst. of Chemistry, [email protected]

2 Photonion GmbHSchwerin, [email protected]

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Content

1. Photo ionisation mass spectrometry (PIMS) in tobacco or nicotine product smoke/vapour on-line analysis

2. Photo ionisation mass spectrometry concept for analysis of aldehydes and other toxicants in e-cigarettes

3. Photo ionisation mass spectrometry concept for analysis of toxicants in tobacco heating products

4. Outlook, summary and conclusion

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PIMS - Soft photo ionisation in vacuum (no fragmentation as in EI-MS and no matrix effects as in CI-MS) direct MS analysis

Two photo ionisation techniques of different selectivity are applied:

IE

Sn

S0

REMPI

b) Resonance-Enhanced Multiphoton Ionisation (REMPI)- ionisation by UV laser pulses (210-270 nm, ~107 W/cm2) - highly efficient soft two-photon ionization of aromatics- ppb/ppt on-line concentration range

IE

S0SPI

a) Vacuum UV Single Photon Ionisation (SPI)- ionisation with 118 nm laser photons (10.5 eV) or

incoherent VUV radiation (excimer lamp, e.g. 9.8 eV)- soft ionization of most organic compounds- ppb on-line concentration range

Mass analysis by time-of-flight (TOFMS), ion trap (ITMS) etc.

Introduction: Photo ionization - SPI and REMPI

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Tobacco smoke (2R4F)

Introduction: Photo ionization - SPI and REMPI

N2

S.Mitschke, W.Welthagen R.Zimmermann, Anal.Chem. 78 (2006) 6364-6375T.Adam, S.Mitschke, T.Streibel, R.R.Baker , R.Zimmermann, Chem. Res. Toxicol. 19 (2006) 511-520

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PI-MS for time- and space-resolved chemical mapping: Distribution maps (middle of puff)

Zimmermann, R.; Hertz-Schünemann, R.; Ehlert, S.; Liu, C.; McAdam, K.; Baker, R.; Streibel, T. Analytical Chemistry 2015, 87, 1711–1717

Hertz-Schünemann, R.; Ehlert, S.; Streibel, T.; Liu, C.; McAdam, K.; Baker, R. R.; Zimmermann, R.. Analytical and Bioanalytical Chemistry 2015

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Photo ionization – mass spectrometry:On-line tobacco smoke analysis

Photo ionization MS smoke profiler forIndustrial applications (Borgwaldt KC)

Stand-alone photo ionization MS forflexible applications (Photonion GmbH)

• Easy to use integrated smoke machine-PI-mass spectrometer system

• Compact oa-TOFMS mass analyzer (R~900)• Different VUV-lamps for SPI + EI ion source• Specific software solution

• High flexibility and sensitivity• Direct Reflectron TOF mass analyzer (R~2000)• REMPI, laser-SPI and VUV lamp SPI source• EI ion source and switchable ionization• Multiple coupling options, custom made software

• Integrated smoke machine – SPI-TOFMS system ( ISO, intense, human, e-cig. profiles) for industrial routine & research

• Quantitative puff-resolved on-line analysis of tobacco smoke toxicants (e.g. isoprene, butadiene, benzene) and of e-cigarette and heat-not-burn product smoke composition

• Flexible, ultra-high performance PI-TOFMS system for research and industrial process analysis

• System can be coupled to:- Thermal analysis, - µ-probe sampling device, - Smoking machine (e-cig./HnB),- Human smoking analyzer (Gas/PM) - Smoke particle matter analyzer- Fast gas chromatography pre-

separation (puff-resolved)

General information on e-cigarette and heat not burn SPI/REMPI-TOF analysis tests

Mass spectrometer: Photonion LASER TOF : 118 nm (10.5eV) SPI or 266 nm REMPI

Smoke machine: Borgwaldt LM1

Smoke protocol:human smoking profiles replayed SA7 (~80-112 ml, e-cig) orISO & modified intense (HnB)

Transfer line temp: 200°C

TOFMS Acquisition rate: 10 Hz

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p

Normalized SPI-TOFMS mass spectra of cigarette, e-cigarette & heat-not-burn devices

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~ bell shaped

~ constant

linear increasing

linear increasing

normal cigarettecharcoal heated HnB device

e-cigarette Electrical heated pod HnB device

Puff resolved SPI-MS analysis of nicotine release of cigarette, e-cigarette & heat-not-burn devices

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Main components (Laser-SPI) of e-cigarette smoke (Type I, no nicotine) Aerosolizer compounds: Glycerol and propylene glycol

e-cigarette (refillable with flavor containing reservoirs, puffing triggered vaporizer)

76

45

76

45

45

45

7676

60

60 60

60

SPI-TOFMS e-cigarette analysis (Type I, reusable, automatic activation)

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R. Zimmermann et al. TSCR Conference, Naples, Florida/USA, September 20th- 23rd 2015e-cigarette I (refillable with flavor containing reservoirs, puffing triggered vaporizer)

m/z

Main components (Laser-SPI) of e-cigarette smoke (Type I, no nicotine) Aerosolizer compounds: Glycerol and propylene glycol+ aroma (simple flavour

compound mixture)C6H14O

SPI-TOFMS e-cigarette analysis (Type I, reusable, automatic activation)

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4460/61/62

74

74

162

16256

56

156

138-H2OGlycerol: 44, 56, 61, 74

Main components (Laser-SPI) of e-cigarette smoke (Type II) Aerosolizer compounds: Glycerol, nicotine and menthol

60/61/6244

SPI-TOFMS e-cigarette analysis (Type II, reusable, automatic activation)

[Menthol-H2O]138

e-cigarette (refillable with nicotine/flavor containing reservoirs, puffing triggered vaporizer)

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http://commons.wikimedia.org/wiki/File:Menthol_neutral.svg





156 138 m/zmenthol

162 m/znicotine

menthol

glycerol

acetaldehyde+ glycerol fragment

nicotine

Laser-SPI: Puff profiles (menthol)

e-cigarette (refillable with nicotine/flavor containing reservoirs, puffing triggered vaporizer)

92 74glycerol

SPI-TOFMS e-cigarette analysis (Type II, reusable, automatic activation)

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http://commons.wikimedia.org/wiki/File:Nikotin_-_Nicotine.svg

http://commons.wikimedia.org/wiki/File:Nikotin_-_Nicotine.svg


17.5 ml/s

Particle filter

Flow meter

Smoking pump

Smoking valve

Heated transfer line (250°C)

Samplingpump

Flow meter

Cambridge filter holder

2.5 ml/s

6-port, 2-position switching valve

Analytical column IL-59 (10 m, 0.25 mm, 0.2 µm)

6

3

1

2

5

4

SPI-TOFMSSPI-TOFMS

ISO smoking:one puff (2 s, 35ml) per min

Isomer separation: On-line, puff-resolved GC-SPI-MS analysis of cigarette smoke

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puff 1 puff 2 puff 3 puff 4

SPI-TOFMS on-line measurement 162 m/z (nicotine trace)

1st GC Measurement 2nd GC Measurement 3rd GC Measurement

Isomer separation: On-line, puff-resolved GC-SPI-MS analysis of cigarette smoke

M.Eschner, I.Selmani, T.Gröger, R.Zimmermann, Anal. Chem., 2011, 83, 6619–6627

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Eclipse Ploom IQOS

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke

Tobacco extract pod

Battery

Heat source

Mouth piece

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General informationTOFMS: Photonion Laser TOFSmoking machine: Borgwaldt LM1 Smoke protocol: * ISO 3308:1991 or* modified intense profile (50 ml/30 sec) Transfer line temp: 200°CIon source: 10.5 eV laser SPI

ISO 3308:199135 ml (2s) every 60 s

Intense HnB/e-cig-profile (I-profile)50 ml (3s) every 30 s

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Puff profiles

59 60 61 62 63 640

5

10

15

20

25

30

35

40

Flow

Time in s

intern lab ISO

0 60 120 180 660 720 780 8400

5

10

15

20

25

30

35

40

Flow

Time in s

intern lab ISO

intense intense

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60/61/62

Heat not burn cigarette I (charcoal heated tobacco vaporizer)

Aerosolizer: Glycerol

SPI-TOFMS heat-not-burn device analysis (Eclipse, charcoal heated system, overview MS)

+ tobacco compounds

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dehydrated

Aerosolizer: Propylene glycol

SPI-TOFMS heat-not-burn device analysis (Ploom, electrical heated pod system, overview MS)

Heat not burn cigarette II (electrical heated tobacco pod vaporizer)

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SPI-TOFMS heat-not-burn device analysis (IQOS, electrical heated tob. rod system, overview MS)

Heat not burn cigarette II (electrical heated tobacco pod vaporizer)

60/61/62

Aerosolizer: Glycerol+ tobacco compounds

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0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170

1E-4

1E-3

0,01

0,1

0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170

1E-4

1E-3

0,01

0,1

0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170

1E-4

1E-3

0,01

0,1

1

0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170

1E-4

1E-3

0,01

0,1

signa

l inte

nsity

in V

IQOS Eclipsesig

nal in

tens

ity in

V

m / z

Ploom

m / z

Research Cigarette

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Complexity profile

Eclipse

Ploom 2R4F Reference cig.

IQOS

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SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Nicotine profiles

Puff profiles matter for nicotine delivery ! This supports the necessity of on-line measurements for HnB and e-cig

I-Profile ISO-Profile

Eclipse

Ploom

IQOS

Reference

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SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Integrated Nicotine profiles

Pod-HnB device (Ploom) best reproduces cigarette nicotine pattern!

I-Profile ISO-Profile

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0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,000

0,005

0,010

0,015

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,00

0,05

0,10

0,15

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,000

0,005

0,010

0,015

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32

0,5

1,0

1,5

IQOS Phenol

inte

grat

ed S

igna

l Eclipse Phenol

Ploom Phenol

Puff

Research Cigarette Phenol

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 321

2

3

4

IQOS Nicotine

inte

grat

ed S

igna

l Eclipse Nicotine

Ploom Nicotine

Puff

Research Cigarette Nicotine

reduction > 10000

reduction ~ 10

reduction ~ 500

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Phenol

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0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 321

2

3

4

IQOS Nicotine

inte

grat

ed S

igna

l Eclipse Nicotine

Ploom Nicotine

Puff


0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,5

1,0

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320

1

2

3

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 3202468

10

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320

5

10

15

20

IQOS Acetaldehyde

inte

grat

ed S

igna

l

Eclipse Acetaldehyde

Ploom Acetaldehyde

Puff

Research Cigarette Acetaldehyde

reduction ~ 2

reduction ~ 10

reduction ~ 20

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Acetaldehyde

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0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 321

2

3

4

IQOS Nicotine

inte

grat

ed S

igna

l Eclipse Nicotine

Ploom Nicotine

Puff


0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,000

0,002

0,004

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,00

0,01

0,02

0,03

0,04

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,000

0,002

0,004

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320

1

2

3

4

IQOS Benzene

inte

grat

ed S

igna

l Eclipse Benzene

Ploom Benzene

Puff

Research Cigarette Benzene

reduction ~ 5000

reduction ~ 50

reduction > 5000

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Benzene

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0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 321

2

3

4

IQOS Nicotine

inte

grat

ed S

igna

l Eclipse Nicotine

Ploom Nicotine

Puff


0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0000

0,0005

0,0010

0,0015

0,0020

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,00

0,05

0,10

0,15

0,20

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0000

0,0005

0,0010

0,0015

0,0020

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 322

4

6

8

IQOS Furan

inte

grat

ed S

igna

l Eclipse Furan

Ploom Furan

Puff

Research Cigarette Furan

reduction ~ 10000

reduction ~ 50

reduction ~ 10000

IsoprenIsoprene

Isoprene

Isoprene

Isoprene

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Isoprene

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0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,1

0,2

0,3

0,4

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 321

2

3

4

IQOS Nicotine

inte

grat

ed S

igna

l Eclipse Nicotine

Ploom Nicotine

Puff


0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,000

0,005

0,010

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,00

0,01

0,02

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,000

0,005

0,010

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 320,0

0,5

1,0

1,5

IQOS Butadiene

inte

grat

ed S

igna

l Eclipse Butadiene

Ploom Butadiene

Puff

Research Cigarette Butadiene

reduction ~10000

reduction > 50

reduction ~ 10000

SPI-TOFMS for on-line analysis of Heat-not-Burn tobacco product smoke: Butadiene

Harm reduction: HnB drastically reduces small, toxic combustion by-products

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Summary

• PI-MS (REMPI, SPI): On-line method for real-time analysis of trace gases, aerosolizer, aroma cpds. & pyrolysis products

• Analysis of e-cig. vapors: Puff-resolved detection of acet-aldehyde, glycerol, propylene glycol, flavors, nicotine etc.

• For aldehyde quantitation on-line GC - PI-MS

• Analysis of HnB-smoke: Puff-resolved detection of tobacco compounds and aerosolizer-compounds

• Massive reduction of gaseous toxicants and tar-compounds• Strong influence of puff-profile, device, age of material etc. on-line measurement required

• Spin-off company Photonion GmbH: Custom-build PI-MS Systems for Research and Cooperation with Borgwaldt KC

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Zimmermann group @Joint Mass Spectrometry Centre AcknowledgementsDr. J. MaguhnDr. T. StreibelDr. J. Schnelle-KreisDr. M. SklorzDr. J. LintelmannDr. E. FeichtDr. M. KirchnerDr. P. RichthammerDr. J. PassigDr. G. JakobiDr. S. SmitaDr. J. OrascheDr. G FerronDr. S. HaackDr. S. EhlertE. HübnerT. GrögerT. MierschA. SutherlandS. Ly-VerduS. WohlfahrtM. FischerC. RügerT. SchwemerG. DraganH. CzechV. Kohlmeier Y. GiessenJ. Parra

S. ErdmannB. WegglertS. OttoS. KrügerP. SattlerG. AbbazadeM. OsterE. KargB. GruberM. JennerweinF. LiL. MüllerA. RhedaX. WuS. ScholtesC. RadischatL. MüllerK. LauM. HahnY. HuangG. KocsisJ.VargaS. ScholtesC. KühlR.ReissM. OsterM. Fuchs

Joint Mass Spectrometry CentreFunding:• Uni Rostock und Helmholtz Zentrum München• Deutsche Forschungsgemeinschaft (DFG)• Bundesministerium für Bildung &Forschung (BMBF)• Bayerische Forschungsstiftung (BFS)• Deutsche Gesetzl. Unfallversich. (DGUV)• Bundeskriminalamt (BKA)• Companies (SASOL Ltd., Netzsch GmbH, Photonion GmbH,

Airsense GmbH, Borgwaldt KC etc.)• Helmholtz-Impulse and Networking- Fonds

(Virtual Helmholtz Institute - HICE)

Dr. S.Ehlert

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Documents

On-line real-time analysis of e-cigarette vapors and heat-not-burn tobacco … · 2018-02-16 · R. Zimmermann et al. TSCR Conference, Naples, Florida/USA, September 20th- 23rd 2015