E-Vapour (EVAP) Sub-Group 2017 Report · 2017 084 Aerosol Collection Strategies for E-Cigarette ... May 2017 Discuss results at 2017 Spring EVAP meeting ... Research Institute of

Kitzbühel, Austria – October 10, 2017

E-Vapour (EVAP) Sub-Group

2017 Report

Evolution

o 2014, formation of E-cigarette TF

o 2016, TF activities completed; formation of E-vapor product

SG

2

History

EVAP SG Report

SSPT2017, Kitzbühel - 171010

SG Coordinator

o Charles Garner - RAISC

SG Secretary

o Gene Gillman – Enthalpy Analytical

SG membership

o ≈ 50 people US, EU, Asia

o E-Vapour Product Companies, Suppliers, Contract Labs,

Regulatory Agencies, Academia, Others, …...

3

E-Vapour Products SG Membership

EVAP SG Report


Scope:

1) To identify areas of scientific research and conduct studies that

will characterize liquids, e-vapour product emissions, and device

properties and performance

2) To develop and publish methods and guides

3) To organize and conduct periodic proficiency/collaborative

studies of identified constituents in liquids and/or e-vapour

product aerosol

4

E-Vapour Product Sub-Group

EVAP SG Report


Technical Guidelines

1) No. 18 - Sample Handling and Sample Collection of

E-Cigarettes and E-Vapour Generating Products -- Published on CORESTA Website November on 2016

5

Accomplishments

EVAP SG Report


Technical Reports

1) Preliminary Proficiency Study for Analysis of Nicotine,

Glycerin, PG, and Water in e-cigarette aerosol

To be published on CORESTA Website by October 2017

2) 2015 Collaborative Study for Determination of Glycerin,

Propylene Glycol, Water and Nicotine in Collected Aerosol of

E-Cigarettes

Was published on CORESTA Website on March 2017

6

Accomplishments

EVAP SG Report


CORESTA Recommended Methods (CRMs)

1) CRM 81 – Routine Analytical Method for E-cigarette Aerosol

Generation & Collection

Was published on CORESTA Website on June 2015

2) CRM 84 - Determination of Glycerin, Propylene Glycol,

Water, and Nicotine in the Aerosol of E-Cigarettes by Gas

Chromatographic Analysis

Was published on CORESTA Website on March 2017

7

Accomplishments

EVAP SG Report


Presentations

Global Tobacco and

Nicotine Forum in Warsaw

Poland June 2017.

Presented on our 2015

Collaborative Study for

Measuring Nicotine,

Glycerin, PG, and Water for

e-vapour products.

8 EVAP SG Report


Active NWIPs

9

E-Vapour Sub-Group

EVAP SG Report


Project

No. Activity Leader Time

127 Carbonyls in e-liquids Melvin 2017

128

Proposed criteria have been circulated in SG that are

being discussed and revised for criteria that should be

considered when selecting an Intense Vaping Regime

Walele

Sinclair

Garner

2017

084 Aerosol Collection Strategies for E-Cigarette

Technologies – Technical Guide

Davis/Joza 2017 (Under

revision by

SG)

088 Comparison of Puffing Parameters – Peer-Reviewed

Publication

EVAP SG 2017

CRM84 specifies technical requirements for the analysis of glycerin,

propylene glycol, nicotine, and water in trapped e-cigarette aerosol

Puffing parameters to collect e-cigarette aerosol

o Puff Volume (55 cc), puff duration (3 sec), puff interval (30 sec), puff

profile (square wave)

Test atmosphere variability

o Temperature ± 2 C

o Relative Humidity ± 5 %

10

Highlights of CRM84

EVAP SG Report


11

Method Summary

EVAP SG Report


Collection • Aerosol collection by CORESTA CRM 81

• 55mL puff, 3s duration, 2x/min, square profile

• Humidity controlled to ± 5%

• Temperature controlled to ± 2 °C

Sample Prep • Pad extraction with Propan-2-ol, 20mL and mechanical shaking

Analysis • GC-TCD for water

• GC-FID for other analytes

• DB-ALC1 30m x 0,32mm x 1,8µm

Active NWIP

Carbonyl Method

List of Carbonyls

Formaldehyde

Acetaldehyde

Acrolein

Crotonaldehyde

Propionaldehyde

Acetone

Butyraldehyde

MEK

Diacetyl

Acetyl Propionyl

Acetoin

13 EVAP SG Report


Study Coordinator - Matt Melvin

Statistical Analysis - Mike Morton

Method Selection from LC/MS, GC/MS, & HPLC – End of November 2016

Approved Study Protocol – Phase I (January 2017) & Phase II (Fall 2017)

Phase I – Liquid (May 2017)

Phase II – Emissions (Fall 2017)

Liquid manufacturers & (16) Laboratories volunteered

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Carbonyl Method

EVAP SG Report


15

Carbonyl Timeline

EVAP SG Report


Date Activity

December 31, 2016 Participants select initial method.

January 13, 2017 Distribute draft protocol, method, and data

reporting sheet

January 20, 2017 Laboratories state their intention to participate

and order supplies

January 27, 2017 Distribute final protocol, method, and data

reporting sheet

End January to

February 17, 2017 Participants order and receive the samples

February – March

31, 2017 Laboratories conduct the study

April 1, 2017 Laboratories submit results by this date

April 2017 Statistical evaluation and preparation of results

May 2017 Discuss results at 2017 Spring EVAP meeting

17 laboratories from 8 countries agreed to participate

Received 10 datasets

16

Participating Laboratories

EVAP SG Report


Participating Laboratories

Essentra Scientific Labstat International ULC Lauterbach & Associates

ASL Analytic Service

Laboratory GmbH JTI UK

Shanghai New Tobacco Products

Research Institute of CNTC

R.J. Reynolds Tobacco Global Laboratory Services Laboratoire National de Métrologie

et D'essais

Zhengzhou Tobacco

Research Institute of CNTC Altria Client Services KT&G Research Institute

JTI Oekolab Enthalpy Analytical Inc – RDU Swisher International, Inc.

JAPAN TOBACCO INC. Enthalpy Analytical Inc. –RVA

Technical Report circulated to SG

R values between 18% to >200%

Follow-up stability study on the test samples found that carbonyl

compounds are not stable when added to e-liquids

It is not possible to evaluate method performance using a

collaborative study using shared samples

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Carbonyl Method

EVAP SG Report


0

20

40

60

80

100

120

0 10 20 30 40

% F

rom

Tim

e Z

ero

Days

Tobacco Flavored E-liquid

Acetoin

Acetone

2-Butanone

Acetaldehyde

Propionaldehyde

Butyraldehyde

Diacetyl

Formaldehyde

Pentanedione

Crotonaldehyde

Acrolein

18

Stability of carbonyls in e-liquids

EVAP SG Report


Intense Vaping Regime(s)

‘Premarket Tobacco Product Applications for

Electronic Nicotine Delivery Systems’

Lines 1021 – 1024

“Evaluating new tobacco products under a range of conditions,

including both non-intense (e.g., lower levels of exposure and

lower volumes of aerosol generated) and intense (e.g., higher

levels of exposure and higher volumes of aerosol generated),

enables FDA to understand the likely range of delivery of

emissions”

20

Intense Vaping Regime

EVAP SG Report


Scientific justification for an intensive vaping regime

will be determined based on the following factors:

1. Vaping topography data

2. Learnings from existing data assessing different vaping

parameters

3. Technical constraints of vaping devices and smoking

machines

21


EVAP SG Report


Vaping Topography: Mean puff durations did not exceed 6 seconds

22


EVAP SG Report


Vaping Topography: Majority of inter-puff intervals below 30 seconds

23


EVAP SG Report


Vaping Topography: Mean puff volumes ranged approx. 50 – 200 mL

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EVAP SG Report


Learnings from existing data assessing vaping parameters

o Puff duration is the major factor impacting e-cigarette delivery

o Puff volume has minimal to no impact on e-cigarette delivery

Technical constraints of vaping devices and smoking machines

o Number of issues reported for some products using a bell shape puff profile

o Device failure issues reported for some products if the flow rate was not

sufficient for device activation (no known issues with CRM81 flow rate of

18.3 mL/s = 55 mL / 3 seconds)

o Smoke machine modifications may be required for puff volumes >70 mL and

inter-puff intervals <30 seconds

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EVAP SG Report


Should the group recommend an intense regime, or provide

guidance on how to choose one?

Is the inter-puff interval (30 seconds) appropriate? Should this be

specified in the document, or provide guidance on how to select one?

Is the puff duration (5 seconds) appropriate? Should this be specified in

the document, or provide guidance on how to select one?

Is the puff volume (95 ml) appropriate or needed? Should this be

specified in the document, or provide guidance on how to select one?

26


EVAP SG Report


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Next Steps

EVAP SG Report


Update during meeting.

Carbonyls in e-liquid

Complete Tech Report

At this time we will not draft a CRM. Aerosol results will be used to support a

CRM.

Carbonyls in aerosol-Lead Melvin

Group supports collaborative study

More work is need to better define the study samples

Small group to test devices and follow-up with the group.

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Next Steps

EVAP SG Report


Update during meeting.

Metals: Lead Joza and Colton

Proficiency study with in-house methods

Follow-up email to group once the timeline is set and protocol drafted

Stability indicating compounds: Walele, Dull, Miller, Joza and Davis

First step: Guidance document on conduct of a stability study

Follow-up at the next meeting to define next steps.

Questions?

Documents

E-Vapour (EVAP) Sub-Group 2017 Report · 2017 084 Aerosol Collection Strategies for E-Cigarette ... May 2017 Discuss results at 2017 Spring EVAP meeting ... Research Institute of