SIST EN 16521:2014

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



SIST EN 16521:2014



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.
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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



EN 16521:2014 (E) 2 Contents Page Foreword .3 Introduction .3 1 Scope .5 2 Reagents .5 3 Apparatus and equipment .6 4 Procedure .6 4.1 Standard purity .6 4.2 Sample preparation .7 4.3 Gas chromatography (GC) measurement conditions .7 4.4 Detection .8 4.4.1 General .8 4.4.2 MS detection in Selected Ion Monitoring (SIM) mode .8 5 Evaluation .9 5.1 Identification and quantitative determination .9 5.2 Calculation . 10 6 Test report . 10 Annex A (informative)
Example of Chromatograms . 11 Bibliography . 12
SIST EN 16521:2014



EN 16521:2014 (E) 3 Foreword This document (EN 16521:2014) has been prepared by Technical Committee CEN/TC 392 “Cosmetics”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2014 and conflicting national standards shall be withdrawn at the latest by November 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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 the United Kingdom. SIST EN 16521:2014



EN 16521:2014 (E) 4 Introduction Phthalates are esters of phthalic acid (Figure 1). About 80 % of all phthalates manufactured are used as “plasticizers” to make plastics flexible without sacrificing strength or durability. These compounds are present in cosmetic products like perfumes and toiletries. Some phthalates, particularly those of low molecular weight, are introduced into cosmetics as ingredients, for examples DEP and DMP are used as solvents and perfume fixatives [1-3] or DEP can be used as alcohol denaturing [2, 4]. Their presence in such products may come from their use as ingredients during the manufacturing process or may come from the migration of phthalates from packaging when plastic is used. Their presence as contaminant could also be due to the manufacturing process or raw materials used. Some analytical methods are proposed in the literature for the determination of phthalates in cosmetic products [1, 4-12].
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



EN 16521:2014 (E) 5 1 Scope 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. 2 Reagents If not otherwise specified, analytical-grade chemicals shall be used. 2.1 Phthalates considered Table 1 — Phthalates considered Phthalates CAS Manufacturerb Quality DBP a
(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



EN 16521:2014 (E) 6 Weigh approximately 10 mg of 4,4-Dibromodiphenyl (2.3) into a 10 ml volumetric flask. Firstly, dissolve in a small amount of ethanol (2.2) and then fill to the calibration mark with ethanol. This stock solution is daily prepared. 2.5 Phthalates stock solution, c = 500 µg/ml (SM). Weigh approximately 10 mg of each phthalate (2.1) into a 20 ml volumetric flask. Firstly, dissolve in a small amount of ethanol (2.2) and then fill to the calibration mark with ethanol. This stock solution has a shelf life of at least 2 weeks if stored in a refrigerator. NOTE Due to the low amount of DIPP standard (sold in quantities of 10,0 mg), a stock solution of this phthalate is prepared independently from other phthalates. In this way, two intermediate stock solutions SM-1 and SM-2 at 1 000 µg/ml are prepared. SM-1 is prepared weighting approximately 10 mg of each phthalate (2.1), except DiPP, into a 10,0 ml volumetric flask, whereas SM-2 is prepared weighting approximately 5,0 mg of DiPP (2.1) into a 5,0 ml volumetric flask. The final stock solution SM is obtained mixing equal volumes of both standard solutions (c = 500 µg/ml). All these stock solutions have a shelf life of at least 2 weeks if stored in a refrigerator. 2.6 Calibration solutions (standard solutions) 1,0 ml of the phthalate stock solution SM (2.5) is transferred into a 10,0 ml volumetric flask and filled with ethanol (2.2) up to the calibration mark (c = 50 5 calibration solutions are prepared by dilution in ethanol (2.2) after the addition of 100 µl of the internal standard stock solution (SM-ISTD). Phthalates concentrations on these cal
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