1、 ISO 2017 Cosmetics Analytical method Detection and quantitative determination of Diethanolamine (DEA) by GC/MS Cosmtique Mthode analytique Dtection et dosage quantitatif de la dithanolamine (DEA) par CG/SM TECHNICAL REPORT ISO/TR 18818 Reference number ISO/TR 18818:2017(E) First edition 2017-06 ISO
2、/TR 18818:2017(E)ii ISO 2017 All rights reserved COPYRIGHT PROTECTED DOCUMENT 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 photo
3、copying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22
4、 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.org ISO/TR 18818:2017(E)Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 T erms 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
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 DE
6、A .5 Bibliography 7 ISO 2017 All rights reserved iii Contents Page ISO/TR 18818:2017(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
7、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 coll
8、aborates 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 appro
9、val 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 th
10、e 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).
11、 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 IS
12、Os 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 ISO/TR 18818:2017(E) Introduc
13、tion 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).
14、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 matrices have been developed and published 1 2 3 . Among the methods available for the analysis of alk
15、anolamines, techniques using gas chromatography (GC) or liquid chromatography (LC) with a variety of detector systems have received the most attention 4 5 . More recent procedures, mass spectrometry (MS) detection in combination with chromatography separation is used to determine analyte content in
16、aqueous solutions with minimal requirements for extraction and cleanup. 6 7In some cases, derivatization of alkanolamines has also been used to improve the chromatographic separations and detection 8 9 . This document describes a rapid and simple method suitable for simultaneously qualitative and qu
17、antitative screening of cosmetics and cosmetic raw materials containing residue of above 0,1 % diethanolamine (DEA). ISO 2017 All rights reserved v Cosmetics Analytical method Detection and quantitative determination of Diethanolamine (DEA) by GC/MS 1 Scope This document describes a screening method
18、 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 unfamilia
19、r 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 unus
20、ual 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 normative references in this document. 3 T erms a nd definiti ons No terms and definitions are listed in this document. I
21、SO and IEC maintain terminological databases for use in standardization at the following addresses: ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp IEC Electropedia: available at h t t p :/ www .electropedia .org/ 4 Principle The analyte is extracted with anhydrous ethanol f
22、rom the sample matrix by ultrasonic extraction. Following ultrasonic treatment, the extract is separated from non-soluble compounds by centrifugation treated with anhydrous sodium sulfate (Na 2 SO 4 ), and filtered. The extract thus obtained is then ready for final identification and the quantificat
23、ion with GC-MS. Qualitative results are based on retention timeand confirmed by mass spectrometry. A calibration curve prepared from external standards is then used for quantitative analysis. TECHNICAL REPORT ISO/TR 18818:2017(E) ISO 2017 All rights reserved 1 ISO/TR 18818:2017(E) 5 Procedure 5.1 Pr
24、eparation of calibration solutions 5.1.1 Stock solution A DEA stock solution (5 000 g/ml) is prepared by weighing accurately about 0,5 g of DEA in a 100 ml volumetric flask), dissolving it in ethanol and diluting to the mark. Transfer the stock standard solution into a polytetrafluoroethylene (PTFE)
25、-sealed screw-cap bottle and store in a dark place at a temperature of about 4 C. Alternatively, stock solution of DEA may be purchased as certified solutions. 5.1.2 Standard solution Prepare one intermediate standard solution of 1 000 g/ml by pipetting 20 ml of stock solution (5.1.1) to a 100 ml vo
26、lumetric flask and diluting to the mark with ethanol. Transfer the standard solution into a polytetrafluoroethylene (PTFE)-sealed screw-cap bottle and store in a dark place at a temperature of about 4 C. Standard solutions are stable for 2 w but should be checked regularly for signs of degradation o
27、r evaporation and again just prior to preparing calibration standards from them. 5.1.3 Calibration solutions Prepare calibration solutions by successive dilutions of the standard solution (5.1.2) according to Table 1. Transfer 5,0 ml, 4,0 ml, 3,0 ml, 2,0 ml, 1,0 ml or 0,5 ml of the stock standard so
28、lution to a series of 10 ml volumetric flasks and bring up to reference level with ethanol. These solutions contain, respectively, 500 g/l, 400 g/ml, 300 g/ml, 200 g/ml, 100 g/ml or 50 g/ml DEA in ethanol. Transfer the calibration solutions into polytetrafluoroethylene (PTFE)-sealed screw-cap bottle
29、s and store in a dark place at a temperature of about 4 C. Table 1 Preparation of calibration solutions Calibration solutions C1 C2 C3 C4 C5 C6 C7 Volume of the standard solution added/ml 0 0,5 1,0 2,0 3,0 4,0 5,0 Final volume/ml 10 10 10 10 10 10 10 The approximate concentration of DEA a /(g/ml) 0
30、50 100 200 300 400 500 NOTE Calibration solutions are stable for 1 w. aThe precise concentration of DEA is obtained by the calculation with the mass of DEA. 5.2 Sample preparation Weigh accurately about 1,0 g of the sample to a 10 ml volumetric flask. Add 5,0 ml ethanol and extract for approximately
31、 15 min using ultrasonic treatment. Then bring the total volume to 10 ml with ethanol and centrifuge at 6 000 r/min for 10 min. Take the supernatant in a fresh tube, add 1,5 g of anhydrous sodium sulfate, and filter the collected solution through a 0,45 m filter membrane into a vial for analysis. 5.
32、3 Analysis 5.3.1 General The samples, including the quality control samples, are analysed by GC-MS.2 ISO 2017 All rights reserved ISO/TR 18818:2017(E) 5.3.2 Example of instrumental conditions Injection volume: 1 l, split injection, split ratio 30:1 Column: 6 % cyanopropylphenyl stationary phase colu
33、mn such as Agilent Jc is the concentration of DEA measured according to the standard working curve, g/ml;V is the final volume of the sample solution, ml;m is the sample mass, g;D f is the dilution factor if any (if no step dilution used, D f= 1). Results are given with two decimals place. Key Y par
34、k area (quantitative ion: m/z 74) X concentration (g/ml) Figure 1 Calibration curve for DEA by quantitative ion (m/z 74) detection under SIM mode Annex A shows examples of the target ion (m/z 74) and the total ion chromatography of the DEA. 6 Limit of quantifica tion The limit of quantification (LoQ
35、) of this method has been determined at 1 000 mg/kg (0,1 %). Observed detection limits may vary among different samples, depending upon the nature of interferences in the sample matrix and the characteristics of the specific instrumentation used.4 ISO 2017 All rights reserved ISO/TR 18818:2017(E) An
36、nex A (informative) Examples of typical GC-MS chromatogram of standard DEA DEA (9,609 min) Key Y abundance X time Figure A.1 Selected ion (m/z 74) scan chromatogram of DEA at 250 g/ml (with DB-624 column) ISO 2017 All rights reserved 5 ISO/TR 18818:2017(E) Key Y abundance m/z time Figure A.2 Mass sp
37、ectrum of DEA6 ISO 2017 All rights reserved ISO/TR 18818:2017(E) Bibliography 1 Henriks-Eckerman M.I., Suuronen K., J olanki R. Determination of occupational exposure to alkanolamines in metal-working fluids. Ann. Occup. Hyg. 2007, 51 (2) pp. 153160. DOI: 10 . 1 0 9 3 / a n n h y g / m e l 0 7 9 2 P
38、eru K.M., H eadley J. V ., D oucette W.J. Determination of alkanolamines in cattails (Typha latifolia) utilizing electrospray ionization with selected reaction monitoring and ion-exchange chromatography. Rapid Commun. Mass Spectrom. 2004, 18 (14) pp. 16291634. DOI: 10 .1 0 0 2 / r c m .1 5 3 1 3 Hea
39、dley J.V., Fedorak P .M., Dickson L.C. A review of analytical methods for the determination of sulfolane and alkanolamines in environmental studies. J. AOAC Int. 2002, 85 (1) pp. 154162. D O I : 1 0 . 1 0 1 6 / j . c h r o m a . 2 0 0 9 . 0 5 . 0 5 6 4 Li X., Shi J., Chen L. Determination of diethan
40、olamine in cosmetics based on micellar extraction in situ derivatization coupled with high performance liquid chromatography J. Anal. Methods. 2016, 8 pp. 29152922. DOI: 10 .1039/ c6ay00217j 5 Bord N., Crtier G., Rocca J.L. Determination of diethanolamine or N-methyldiethanolamine in high ammonium c
41、oncentration matrices by capillary electrophoresis with indirect UV detection: application to the analysis of refinery process waters J. Anal. Bioanal. Chem. 2004, 380 ( 2 ) p p . 3 2 5 3 3 2 . D O I : 1 0 . 1 0 0 7 / s 0 0 2 1 6 - 0 0 4 - 2 7 5 4 - 3 6 ASTM D7599-09: 2012, Standard test method for
42、determination of diethanolamine, triethanolamine, n-methyldiethanolamine and n-ethyldiethanolamine in water by single reaction monitoring liquid chromatography/tandem mass spectrometry (LC/MS/MS) 7 SN/T 2107-2008, Determination of monoethanolamine, diethanolamine and triethanolamine in cosmetics for
43、 import and export 8 Zacharis C. K. , & T zanavaras P . D . L i q u i d c h r o m a t o gr a p h y c o u p l e d t o o n - l i n e p o s t c o l u m n derivatization for the determination of organic compounds: a review on instrumentation and chemistries. Anal. Chim. Acta. 2013, 798 ( 1 0 ) p p . 1 2
44、 4 . D O I : 1 0 . 1 0 1 6 / j . a c a . 2 0 1 3 . 0 7 . 0 3 2 9 Whiteside I.R.C., Worsfold P . J . , M cKerrell E . H . D e t e r m i n a t i o n o f a l k y l a m i n e s b y h i g h - performance liquid chromatography with post-column fluorescence derivatization. Anal. Chim. Acta. 1988, 212 ( 1 - 2 ) p p . 1 5 5 1 63 . D O I : 1 0 . 1 0 1 6 / S 0 0 0 3 - 2 6 7 0 ( 0 0 ) 8 4 1 3 7 - 9 ISO 2017 All rights reserved 7
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