SIST-TP ISO/TR 18818:2018

Cosmetics - Analytical method - Detection and quantitative determination of Diethanolamine (DEA) by GC/MS

ISO/TR 18818:2017 describes a screening method for rapid sampling and identifying of diethanolamine (DEA) in cosmetics and raw materials used in cosmetics by gas chromatography ? mass spectroscopy (GC-MS).
This method is not applicable to the detection and/or quantification of DEA-related ingredients. When this method is used to analyse unfamiliar sample matrices analysts are advised to confirm the applicability and flexibility of the techniques in their matrix.
Under the conditions specified this method is reliable for quantification with DEA level at 1 000 mg/kg (0,1 %).
However, samples with lower concentrations (

Cosmétique - Méthode analytique - Détection et dosage quantitatif de la diéthanolamine (DEA) par CG/SM

Kozmetika - Analizne metode - Detekcija in kvantitativno določevanje dietanolamina (DEA) s plinsko kromatografijo z masno spektrometrijo (GC/MS)

Ta dokument opisuje presejalno metodo za hitro vzorčenje in prepoznavanje dietanolamina (DEA) v kozmetičnih izdelkih ter surovinah, ki se uporabljajo v kozmetiki, s plinsko kromatografijo – masno spektroskopijo (GC-MS).
Ta metoda se ne uporablja za detekcijo in/ali kvantitativno določevanje sestavin, povezanih z dietanolaminom. Pri uporabi te metode za analizo neznanih vzorčnih matric se analitikom priporoča, da potrdijo uporabnost in prilagodljivost tehnik v svoji matrici.
Ta metoda je pod opredeljenimi pogoji zanesljiva za kvantitativno določevanje z ravnjo dietanolamina 1000 mg/kg (0,1 %).
Vendar vzorci z nižjimi koncentracijami (<0,1 %) ali kako drugače nenavadne sestave ali lastnosti lahko pomenijo težave (kot je na primer razvlečenost vrhov), ki preprečujejo neposredno uporabo te metode.

General Information

• Status: Published
• Public Enquiry End Date: 02-Nov-2017
• Publication Date: 07-Oct-2018
• ICS: 71.040.50 - Physicochemical methods of analysis
• ICS: 71.100.70 - Cosmetics. Toiletries
• Technical Committee: KDS - Cosmetics, chemical disinfectants and surface active agents
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 11-Sep-2018
• Due Date: 16-Nov-2018
• Completion Date: 08-Oct-2018
• Ref Project: ISO/TR 18818:2017 - Cosmetics - Analytical method - Detection and quantitative determination of Diethanolamine (DEA) by GC/MS

Overview

ISO/TR 18818:2017 specifies a rapid screening and quantitative analytical method for detecting Diethanolamine (DEA) in cosmetics and cosmetic raw materials using gas chromatography–mass spectrometry (GC‑MS). It is designed as a simple extraction + GC‑MS workflow for confirmation and quantification of DEA at or above the method’s limit of quantification (LoQ) of 1 000 mg/kg (0.1%). The method is not applicable to DEA‑related ingredients and users must verify applicability for unfamiliar sample matrices.

Key topics and technical requirements

• Scope: Screening and quantification of free DEA in cosmetics/raw materials only; DEA‑related compounds are excluded.
• Sample preparation:
  • Weigh 1.0 g sample and extract with ethanol (5.0 mL), ultrasonic treatment (15 min), bring to 10 mL, centrifuge (≈6 000 r/min, 10 min).
  • Drying agent: add ~1.5 g anhydrous sodium sulfate (Na2SO4) and filter through 0.45 µm membrane prior to GC‑MS.
• Calibration and standards:
  • Stock solution example: 5 000 µg/mL DEA; intermediate 1 000 µg/mL; calibration range example 50–500 µg/mL.
  • Calibration curve based on peak area vs. concentration using the quantitative ion m/z 74 in SIM mode; required correlation coefficient R > 0.990.
  • Typical recovery for spiked samples (100–500 µg) should be ≥ 90%.
• GC‑MS parameters (example conditions):
  • Injection: 1 µL, split 30:1; columns suggested (DB‑624 or Rx‑5 ms type); electron ionization 70 eV; EI scan 28–300 amu; monitoring ions include m/z 74 (quant), 56, 45, 30.
• Limitations:
  • LoQ = 1 000 mg/kg (0.1%). Samples with lower DEA levels, unusual matrices or matrix interferences (e.g., peak tailing) may require alternate methods or confirmatory testing.
• Quantification: Concentration in sample solution combined with final volume, sample mass and any dilution factor yields mass fraction (%) of DEA.

Applications and users

• Quality control and screening in cosmetic formulation and raw‑material testing labs
• Regulatory and safety testing laboratories assessing compliance with jurisdictional DEA restrictions
• Contract analytical laboratories performing GC‑MS screening for manufacturers and suppliers
• Cosmetic R&D when verifying absence/presence of residual DEA in ingredients

Related standards and methods

• ISO/TR 18818:2017 complements other analytical approaches for alkanolamines such as LC‑MS/MS, derivatization‑based HPLC methods and standards referenced in the bibliography (e.g., ASTM D7599‑09, SN/T 2107‑2008). Users may select alternative validated methods when lower LoQ or different matrices are required.

Keywords: ISO/TR 18818:2017, Diethanolamine, DEA, GC‑MS, cosmetics, analytical method, limit of quantification, SIM m/z 74, sample preparation, calibration.

Standards Content (Sample)

SLOVENSKI STANDARD
01-november-2018
.R]PHWLND$QDOL]QHPHWRGH'HWHNFLMDLQNYDQWLWDWLYQRGRORþHYDQMH
GLHWDQRODPLQD'($VSOLQVNRNURPDWRJUDILMR]PDVQRVSHNWURPHWULMR*&06
Cosmetics - Analytical method - Detection and quantitative determination of
Diethanolamine (DEA) by GC/MS
Cosmétique - Méthode analytique - Détection et dosage quantitatif de la diéthanolamine
(DEA) par CG/SM
Ta slovenski standard je istoveten z: ISO/TR 18818:2017
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
71.100.70 .R]PHWLND7RDOHWQL Cosmetics. Toiletries
SULSRPRþNL
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL ISO/TR
REPORT 18818
First edition
2017-06
Cosmetics — Analytical method
— Detection and quantitative
determination of Diethanolamine
(DEA) by GC/MS
Cosmétique — Méthode analytique — Détection et dosage quantitatif
de la diéthanolamine (DEA) par CG/SM
Reference number
©
ISO 2017
© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2017 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Procedure. 2
5.1 Preparation of calibration solutions . 2
5.1.1 Stock solution . 2
5.1.2 Standard solution . 2
5.1.3 Calibration solutions . 2
5.2 Sample preparation . 2
5.3 Analysis. 2
5.3.1 General. 2
5.3.2 Example of instrumental conditions . 3
5.3.3 Recovery . 3
5.3.4 Calibration curve . 3
5.4 Determination . 4
6 Limit of quantification . 4
Annex A (informative) Examples of typical GC-MS chromatogram of standard DEA .5
Bibliography . 7
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 on 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 the following
URL: w w w . i s o .org/ iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 217, Cosmetics.
iv © ISO 2017 – All rights reserved

Introduction
Diethanolamine (DEA) has been restricted for use in cosmetics and personal care products in a
number of jurisdictions due to its potential health risk since residual levels of DEA might react with
other specific ingredients to form the extremely potent carcinogen nitrosodiethanolamine (NDELA).
Therefore, a harmonized method for the screening of DEA in cosmetic raw materials is considered
important.
Numerous methods for the trace analysis of alkanolamines including DEA in different sample
[1] [2] [3]
matrices have been developed and published . Among the methods available for the analysis
of alkanolamines, techniques using gas chromatography (GC) or liquid chromatography (LC) with
[4] [5]
a variety of detector systems have received the most attention . More recent procedures, mass
spectrometry (MS) detection in combination with chromatography separation is used to determine
[6] [7]
analyte content in aqueous solutions with minimal requirements for extraction and cleanup.
In some cases, derivatization of alkanolamines has also been used to improve the chromatographic
[8] [9]
separations and detection .
This document describes a rapid and simple method suitable for simultaneously qualitative and
quantitative screening of cosmetics and cosmetic raw materials containing residue of above 0,1 %
diethanolamine (DEA).
TECHNICAL REPORT ISO/TR 18818:2017(E)
Cosmetics — Analytical method — Detection and
quantitative determination of Diethanolamine (DEA) by
GC/MS
1 Scope
This document describes a screening method for rapid sampling and identifying of diethanolamine
(DEA) in cosmetics and raw materials used in cosmetics by gas chromatography – mass spectroscopy
(GC-MS).
This method is not applicable to the detection and/or quantifica
...

TECHNICAL ISO/TR
REPORT 18818
First edition
2017-06
Cosmetics — Analytical method
— Detection and quantitative
determination of Diethanolamine
(DEA) by GC/MS
Cosmétique — Méthode analytique — Détection et dosage quantitatif
de la diéthanolamine (DEA) par CG/SM
Reference number
©
ISO 2017
© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2017 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Procedure. 2
5.1 Preparation of calibration solutions . 2
5.1.1 Stock solution . 2
5.1.2 Standard solution . 2
5.1.3 Calibration solutions . 2
5.2 Sample preparation . 2
5.3 Analysis. 2
5.3.1 General. 2
5.3.2 Example of instrumental conditions . 3
5.3.3 Recovery . 3
5.3.4 Calibration curve . 3
5.4 Determination . 4
6 Limit of quantification . 4
Annex A (informative) Examples of typical GC-MS chromatogram of standard DEA .5
Bibliography . 7
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 on 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 the following
URL: w w w . i s o .org/ iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 217, Cosmetics.
iv © ISO 2017 – All rights reserved

Introduction
Diethanolamine (DEA) has been restricted for use in cosmetics and personal care products in a
number of jurisdictions due to its potential health risk since residual levels of DEA might react with
other specific ingredients to form the extremely potent carcinogen nitrosodiethanolamine (NDELA).
Therefore, a harmonized method for the screening of DEA in cosmetic raw materials is considered
important.
Numerous methods for the trace analysis of alkanolamines including DEA in different sample
[1] [2] [3]
matrices have been developed and published . Among the methods available for the analysis
of alkanolamines, techniques using gas chromatography (GC) or liquid chromatography (LC) with
[4] [5]
a variety of detector systems have received the most attention . More recent procedures, mass
spectrometry (MS) detection in combination with chromatography separation is used to determine
[6] [7]
analyte content in aqueous solutions with minimal requirements for extraction and cleanup.
In some cases, derivatization of alkanolamines has also been used to improve the chromatographic
[8] [9]
separations and detection .
This document describes a rapid and simple method suitable for simultaneously qualitative and
quantitative screening of cosmetics and cosmetic raw materials containing residue of above 0,1 %
diethanolamine (DEA).
TECHNICAL REPORT ISO/TR 18818:2017(E)
Cosmetics — Analytical method — Detection and
quantitative determination of Diethanolamine (DEA) by
GC/MS
1 Scope
This document describes a screening method for rapid sampling and identifying of diethanolamine
(DEA) in cosmetics and raw materials used in cosmetics by gas chromatography – mass spectroscopy
(GC-MS).
This method is not applicable to the detection and/or quantification of DEA-related ingredients.
When this method is used to analyse unfamiliar sample matrices analysts are advised to confirm the
applicability and flexibility of the techniques in their matrix.
Under the conditions specified this method is reliable for quantification with DEA level at 1 000 mg/kg
(0,1 %).
However, samples with lower concentrations (<0,1 %) or otherwise unusual compositions or
characteristics can present difficulties (such as, for example, peak tailing) that preclude the direct use
of this method.
2 Normative references
There are no normat
...