Cosmetics - Analytical methods - GC/MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection

This European Standard describes a GC/MS method for the assay of 12 phthalates, amongst which the 8 phthalates regulated by the European cosmetic regulation 1223/2009 [16]. This method is given for the analysis of samples ready for analytical injection from cosmetic products or raw materials used in cosmetic products. Samples should be compatible with GC analysis possibly after dilution. This method does not include requirements for the preparation of samples in cosmetic matrices for which direct injection in GC is not feasible.

Kosmetische Mittel - Analysenmethoden - GC/MS-Methode für die Identifizierung und die Quantifizierung von 12 Phthalaten in zur direkten Injektion geeigneten Proben kosmetischer Mittel

Diese Europäische Norm legt ein GC/MS-Verfahren für die Untersuchung von 12 Phthalaten fest, von denen 8 Phthalate durch die europäische Kosmetikverordnung 1223/2009 [16] geregelt sind. Dieses Verfahren ist für die Analyse von zur direkten Injektion geeigneten Proben von kosmetischen Mitteln oder für Rohstoffe, die in kosmetischen Mitteln verwendet werden, anwendbar. Die Proben sollten für die GC-Analyse, möglicherweise nach Verdünnung, geeignet sein. Dieses Verfahren beinhaltet keine Anforderungen an die Probenvorbereitung kosmetischer Matrices, bei denen die direkte Injektion in den GC nicht möglich ist.

Cosmétiques - Méthodes analytiques - Méthode CG-SM pour l'identification et l'analyse de 12 phtalates dans des échantillons de produits cosmétiques prêts à être injectés dans un système analytique

La présente Norme européenne décrit une méthode CG-SM de dosage de 12 phtalates, parmi lesquels sont compris les huit phtalates réglementés par le Règlement européen relatif aux produits cosmétiques 1223/2009 [16]. Cette méthode s'applique à l'analyse d'échantillons prêts à être injectés dans un système analytique et issus de produits cosmétiques ou de matières premières entrant dans la composition de produits cosmétiques. Il convient que les échantillons soient compatibles avec l'analyse par chromatographie en phase gazeuse après une possible dilution. La présente méthode n'inclut pas d’exigences pour la préparation d’échantillons de matrices cosmétiques incompatibles avec une injection directe par chromatographie en phase gazeuse.

Kozmetika - Analizne metode - Metoda GC/MS za identifikacijo in analizo 12 ftalatov v kozmetičnih vzorcih, pripravljenih za neposredno injeciranje

EN 16521 opisuje metodo plinske kromatografije (GC)/masne selekcije (MS) v preskusih 12 ftalatov, med katerimi je 8 ftalatov, ki jih ureja evropska uredba o kozmetičnih izdelkih 1223/2009 [16]. Ta metoda je podana za analizo vzorcev, pripravljenih za analitično injiciranje iz kozmetičnih izdelkov ali surovin, uporabljenih v kozmetičnih izdelkih. Vzorci morajo biti združljivi z analizo s plinsko kromatografijo po možnosti po redčenju. Ta metoda ne vključuje zahtev za pripravo vzorcev v kozmetičnih matricah, za katere neposredno injiciranje v GC ni izvedljivo.

General Information

Status
Published
Publication Date
06-May-2014
Withdrawal Date
29-Nov-2014
ICS
71.100.70 - Cosmetics. Toiletries
Technical Committee
CEN/TC 392 - Cosmetics
Drafting Committee
CEN/TC 392/WG 1 - Analytical methods
Current Stage
9093 - Decision to confirm - Review Enquiry
Start Date
13-Dec-2022
Completion Date
14-Apr-2025
Ref Project
SIST EN 16521:2014 - Cosmetics - Analytical methods - GC/MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection

Overview

EN 16521:2014 is a CEN European Standard that specifies a GC/MS method for the identification and quantitative assay of 12 phthalates in cosmetic samples that are ready for analytical injection. The scope includes the 8 phthalates regulated by the European Cosmetic Regulation (EC) No 1223/2009, and covers samples from finished cosmetic products or raw materials provided they are compatible with direct GC analysis (possibly after dilution). The standard does not define procedures for complex matrix preparation where direct GC injection is not feasible.

Key topics and technical requirements

  • Analytes covered: 12 phthalates (including regulated phthalates such as DMP, DEP, DiBP, DBP, BBP, DEHP, DnOP and others listed in the standard).
  • Instrumentation: Gas chromatography coupled with mass spectrometry (GC/MS) using electron‑impact (EI, 70 eV) ionisation. Full‑scan (m/z 40–350) for identification and Selected Ion Monitoring (SIM) for quantification.
  • Column & oven: Recommended low‑bleed 5%‑phenyl/95%‑dimethylpolysiloxane capillary column (30 m × 0.25 mm × 0.25 µm) with a temperature ramp program supplied in the standard.
  • Internal standard & calibration: Use of 4,4‑dibromodiphenyl as internal standard; calibration solutions typically in the range 0.25–5.0 µg/ml (external calibration or standard addition).
  • Sample preparation: Simple dilution-based prep for samples ready for injection (e.g., 1.0 g sample → 10 ml ethanol with ISTD). Alternative direct vial method for perfumes (1.0 ml + 10 µl ISTD) yields a lower LOQ.
  • Limits of quantification: Method LOQ reported as approximately 5 ppm for the standard sample prep and 0.5 ppm for the direct vial preparation for perfumes.
  • Identification criteria: Retention time matching and characteristic ion ratios (three ions per compound, with tolerances) as documented in the standard.

Applications and users

This standard is intended for:

  • Regulatory and compliance testing labs verifying compliance with EU cosmetic regulation 1223/2009.
  • Cosmetic manufacturers and raw‑material suppliers conducting quality control and incoming material screening.
  • Third‑party contract testing laboratories and forensic or product safety analysts assessing phthalate contamination or migration from packaging.
  • Research groups developing validated GC/MS methods for phthalates in cosmetic matrices.

Practical benefits include harmonised, reproducible procedures for phthalate screening and quantification, guidance on instrument settings (GC program, SIM windows) and validated sample dilution approaches.

Related standards and references

  • EU Cosmetic Regulation (EC) No 1223/2009 - regulatory context for restricted phthalates.
  • ISO 12787 - referenced validation approach used in method development (see EN 16521:2014 bibliography for details).

Keywords: EN 16521:2014, GC/MS method, phthalates in cosmetics, CEN standard, analytical methods, cosmetic regulation 1223/2009, SIM mode, internal standard, limit of quantification.

Frequently Asked Questions

EN 16521:2014 is a standard published by the European Committee for Standardization (CEN). Its full title is "Cosmetics - Analytical methods - GC/MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection". This standard covers: This European Standard describes a GC/MS method for the assay of 12 phthalates, amongst which the 8 phthalates regulated by the European cosmetic regulation 1223/2009 [16]. This method is given for the analysis of samples ready for analytical injection from cosmetic products or raw materials used in cosmetic products. Samples should be compatible with GC analysis possibly after dilution. This method does not include requirements for the preparation of samples in cosmetic matrices for which direct injection in GC is not feasible.

This European Standard describes a GC/MS method for the assay of 12 phthalates, amongst which the 8 phthalates regulated by the European cosmetic regulation 1223/2009 [16]. This method is given for the analysis of samples ready for analytical injection from cosmetic products or raw materials used in cosmetic products. Samples should be compatible with GC analysis possibly after dilution. This method does not include requirements for the preparation of samples in cosmetic matrices for which direct injection in GC is not feasible.

EN 16521:2014 is classified under the following ICS (International Classification for Standards) categories: 71.100.70 - Cosmetics. Toiletries. The ICS classification helps identify the subject area and facilitates finding related standards.

EN 16521:2014 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.LUDQMHKosmetische Mittel - Analysenmethoden - GC/MS-Methode für die Identifizierung und die Prüfung von 12 Phthalaten in kosmetischen Proben für die analytische InjektionCosmétiques - Méthodes analytiques - Méthode GC-MS pour l'identification et le dosage de 12 phtalates dans les produits cosmétiques prêts à être injecté dans un système analytiqueCosmetics - Analytical methods - GC/MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection71.100.70SULSRPRþNLCosmetics. ToiletriesICS:Ta slovenski standard je istoveten z:EN 16521:2014SIST EN 16521:2014en,fr,de01-julij-2014SIST EN 16521:2014SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16521
May 2014 ICS 71.100.70 English Version
Cosmetics - Analytical methods - GC/MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection
Cosmétiques - Méthodes analytiques - Méthode CG-SM pour l'identification et l'analyse de 12 phtalates dans des échantillons de produits cosmétiques prêts à être injectés dans un système analytique
Kosmetische Mittel - Analysenmethoden - GC/MS-Methode für die Identifizierung und die Quantifizierung von 12 Phthalaten in zur direkten Injektion geeigneten Proben kosmetischer Mittel This European Standard was approved by CEN on 10 April 2014.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16521:2014 ESIST EN 16521:2014

Example of Chromatograms . 11 Bibliography . 12
Figure 1 — Esters of phthalic acid This standard proposes a GC/MS method for a simultaneous assay in cosmetic samples ready for analytical injection of 12 phthalates listed in Table 1. These chromatographic conditions are not suitable for the quantification of di-isononyl phthalate (DiNP) or di-isodecyl phthalate (DiDP). According to SCCP [13], the possible presence of DiNP or DiDP in cosmetics does not seem to be a problem for human health. A GC/MS method using positive chemical ionisation with ammonia as collision gas is proposed in literature for the determinations of those compounds in cosmetic products [14]. Analyses are carried out on a GC/MS system with electron impact ionization mode (Ei). The separation of phthalates is obtained on a cross-linked 5 %-phenyl/95 %-dimethylpolysiloxane capillary column 30 m × 0,25 mm (i. d.) × 0,25 µm film thickness using a temperature gradient. Phthalate quantification is performed by external calibration using an internal standard or by the standard addition. Cosmetic samples are analyzed directly or after a previous dilution in ethanol [15]. SIST EN 16521:2014

(dibutyl phthalate) 84–74–2 ALDRICH 97,0 % DEHP a
(diethylhexyl phthalate) 117–81–7 ALDRICH 99,8 % BBP a
(butylbenzyl phthalate) 85–68–7 ALDRICH 97,0 % DMEP a (di(2-methoxyethyl) phthalate) 117–82–8 ALDRICH 97,0 % DnPP a
(di-n-pentyl phthalate) 131–18–0 CIL CLUZEAU 99,0 % DiPP a
(diisopentyl phthalate) 605–50–5 CIL CLUZEAU 95,0 % DPP a
(n-pentyl isopentyl phthalate) 84777–06–0 CIL CLUZEAU 95,0 %* DiBP a
(diisobutyl phthalate) 84–69–5 ACROS 98,0 % DCHP
(dicyclohexyl phthalate) 84–61–7 ALDRICH 98,0 % DEP
(diethyl phthalate) 84–66–2 ACROS 98,0 % DMP
(dimethyl phthalate) 131–11–3 ACROS 98,0 % DnOP
(di-n-octyl phthalate) 117–84–0 ALDRICH 98,0 % a Regulated phthalates. b This is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. * Mixed isomers (DiPP, DnPP and DPP) 2.2 Ethanol 2.3 Internal standard, 4,4-Dibromodiphenyl from Fluka 1) 97,0 % was used as internal standard (ISTD). 2.4 Internal standard stock solution (SM-ISTD), c = 1 000 µg/ml.
1) This is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. SIST EN 16521:2014
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