Cigarettes — Determination of benzo[a]pyrene in cigarette mainstream smoke with an intense smoking regime using GC/MS — Part 1: Method using methanol as extraction solvent

This document specifies a method for the determination of benzo[a]pyrene (B[a]P) in the total particulate matter (TPM) of cigarette mainstream smoke using gas chromatography/mass spectrometry (GC-MS) with methanol as extraction solvent. This method is specified using ISO 20778 smoking parameters. NOTE An alternative method for the determination of B[a]P is specified in ISO 23906-2 with a different clean-up using cyclohexane solvent and a shorter total analytical time.

Cigarettes — Dosage par CG/SM du benzo[a]pyrène dans le courant principal de la fumée de cigarette avec un régime de fumage intense — Partie 1: Méthode utilisant du méthanol comme solvant d'extraction

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Status
Published
Publication Date
29-Sep-2020
Current Stage
6060 - International Standard published
Start Date
30-Sep-2020
Completion Date
30-Sep-2020
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ISO 23906-1:2020 - Cigarettes -- Determination of benzo[a]pyrene in cigarette mainstream smoke with an intense smoking regime using GC/MS
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INTERNATIONAL ISO
STANDARD 23906-1
First edition
2020-09
Cigarettes — Determination
of benzo[a]pyrene in cigarette
mainstream smoke with an intense
smoking regime using GC/MS —
Part 1:
Method using methanol as extraction
solvent
Cigarettes — Dosage par CG/SM du benzo[a]pyrène dans le courant
principal de la fumée de cigarette avec un régime de fumage
intense —
Partie 1: Méthode utilisant du méthanol comme solvant d'extraction
Reference number
ISO 23906-1:2020(E)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 23906-1:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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below or ISO’s member body in the country of the requester.
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Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 23906-1:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Apparatus ..................................................................................................................................................................................................................... 2

6 Reagents ........................................................................................................................................................................................................................ 2

7 Standards ..................................................................................................................................................................................................................... 3

7.1 General ........................................................................................................................................................................................................... 3

7.2 Primary B[a]P stock solution ...................................................................................................................................................... 3

7.3 Secondary B[a]P stock solution ................................................................................................................................................ 3

7.4 B[a]P-d12 stock solution ................................................................................................................................................................ 3

7.5 B[a]P-d12 spiking solution ........................................................................................................................................................... 3

7.6 Working standard solutions ........................................................................................................................................................ 3

7.7 Storage of standard solutions..................................................................................................................................................... 3

8 Preparation of sample .................................................................................................................................................................................... 4

8.1 Sampling ....................................................................................................................................................................................................... 4

8.2 Smoking ......................................................................................................................................................................................................... 4

8.3 Glass-fibre filter pad extraction ................................................................................................................................................ 4

8.4 Sample clean-up ..................................................................................................................................................................................... 4

9 Determination ......................................................................................................................................................................................................... 5

9.1 GC-MS operating conditions ........................................................................................................................................................ 5

9.2 Calibration .................................................................................................................................................................................................. 6

9.3 Determination of B[a]P .................................................................................................................................................................... 6

9.4 Calculation .................................................................................................................................................................................................. 6

10 Repeatability and reproducibility ...................................................................................................................................................... 6

11 Test report ................................................................................................................................................................................................................... 7

11.1 General ........................................................................................................................................................................................................... 7

11.2 Characteristic data about the cigarette .............................................................................................................................. 8

11.3 Data about sampling .......................................................................................................................................................................... 8

11.4 Description of the test ...................................................................................................................................................................... 8

11.5 Test results.................................................................................................................................................................................................. 8

Annex A (informative) Example of a chromatogram of a cigarette smoke extract ...............................................9

Bibliography .............................................................................................................................................................................................................................11

© ISO 2020 – All rights reserved iii
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ISO 23906-1:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco products.

A list of all parts in the ISO 23906 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
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ISO 23906-1:2020(E)
Introduction

Between 1999 and 2003, a task force composed of Cooperation Centre for Scientific Research Relative

to Tobacco (CORESTA) members studied the existing methodologies for the determination of benzo[a]

pyrene (B[a]P) in the mainstream smoke of cigarettes. Several methods have been proposed for this

determination, which are mainly based on two types of analytical methodology: high performance liquid

chromatography (HPLC) with fluorescence detection and gas chromatography/mass spectrometry

(GC-MS). In both cases, it is necessary to purify the total particulate matter (TPM) extract before

performing the chromatography in order to obtain a correct separation of the B[a]P peak.

The task force decided in the first instance to develop a method using HPLC with fluorescence detection.

However, after several collaborative experiments, it appeared that achieving a significant reduction

of the initially observed variability would be technically very difficult. The task force then decided

to investigate a GC-MS method as an alternative and was able to demonstrate, through collaborative

experiments, that a lower variability can be obtained with this methodology.

This document, produced through collaborative experiments conducted in 2012 involving 12

laboratories in 11 countries, provides a procedure for the determination of B[a]P in cigarette

[4]

mainstream smoke. The repeatability and reproducibility of this method have been assessed

according to ISO recommendations and are included.
No machine smoking regime can represent all human smoking behaviours.

— It is recommended that cigarettes also be tested under conditions of a different intensity of machine

smoking than those specified in this document.

— Machine smoking testing is useful to characterize cigarette emissions for design and regulatory

purposes, but communication of machine measurements to smokers can result in misunderstandings

about differences in exposure and risk across brands.

— Smoke emission data from machine measurements may be used as inputs for product hazard

assessment, but they are not intended to be nor are they valid measures of human exposure or

risks. Communicating differences between products in machine measurements as differences in

exposure or risk is a misuse of testing using International Standards.
© ISO 2020 – All rights reserved v
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INTERNATIONAL STANDARD ISO 23906-1:2020(E)
Cigarettes — Determination of benzo[a]pyrene in
cigarette mainstream smoke with an intense smoking
regime using GC/MS —
Part 1:
Method using methanol as extraction solvent

WARNING — The use of this document can involve hazardous materials, operations and

equipment. This document does not purport to address all the safety problems associated with

its use. It is the responsibility of the user of this document to establish appropriate safety and

health practices and determine the applicability of regulatory limitations prior to use.

1 Scope

This document specifies a method for the determination of benzo[a]pyrene (B[a]P) in the total particulate

matter (TPM) of cigarette mainstream smoke using gas chromatography/mass spectrometry (GC-MS)

with methanol as extraction solvent.
This method is specified using ISO 20778 smoking parameters.

NOTE An alternative method for the determination of B[a]P is specified in ISO 23906-2 with a different

clean-up using cyclohexane solvent and a shorter total analytical time.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 3402, Tobacco and tobacco products — Atmosphere for conditioning and testing
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 8243, Cigarettes — Sampling

ISO 20778, Cigarettes — Routine analytical cigarette smoking machine — Definitions and standard

conditions with an intense smoking regime

ISO 20779, Cigarettes — Generation and collection of total particulate matter using a routine analytical

smoking machine with an intense smoking regime
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
© ISO 2020 – All rights reserved 1
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ISO 23906-1:2020(E)
4 Principle

— Sampling of the test cigarettes according to the sampling procedure specified in ISO 8243.

— Conditioning of the test cigarettes according to the conditioning procedure specified in ISO 3402.

— Smoking of the test cigarettes according to the smoking procedure specified in ISO 20779.

— Extraction of the TPM, collected on the appropriate glass-fibre filter pad, with methanol.

— Dilution of the methanol extract with water.

— Loading of the water/methanol solution onto a cyclohexyl solid phase extraction (CH SPE) cartridge,

followed by the elution of B[a]P with cyclohexane.
— Analytical determination of B[a]P by gas chromatography/mass spectrometry.
5 Apparatus
The usual laboratory apparatus and equipment and, in particular, the following.

5.1 Routine analytical cigarette-smoking machine, complying with the requirements of ISO 20778

and equipped for smoking in accordance with ISO 20779.

5.2 Gas chromatograph with a mass selective detector, equipped with its computerized control

and data acquisition and processing system. This system shall be able to pilot the mass spectrometer

in order to obtain chromatographic data under single ion monitoring (SIM) detection mode. The

gas chromatograph shall be configured to perform splitless injections on a capillary column. It is

recommended to equip the gas chromatograph with an autosampler for sample injection.

5.3 Fused silica capillary column, for example a (5 %-phenyl)-methylpolysiloxane stationary phase

and a 30 m length, 0,25 mm intern
...

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