欢迎来到麦多课文档分享! | 帮助中心 海量文档,免费浏览,给你所需,享你所想!
麦多课文档分享
全部分类
  • 标准规范>
  • 教学课件>
  • 考试资料>
  • 办公文档>
  • 学术论文>
  • 行业资料>
  • 易语言源码>
  • ImageVerifierCode 换一换
    首页 麦多课文档分享 > 资源分类 > PDF文档下载
    分享到微信 分享到微博 分享到QQ空间

    DIN EN 16521-2014 Cosmetics - Analytical methods - GC MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection German version .pdf

    • 资源ID:672958       资源大小:872.62KB        全文页数:15页
    • 资源格式: PDF        下载积分:10000积分
    快捷下载 游客一键下载
    账号登录下载
    微信登录下载
    二维码
    微信扫一扫登录
    下载资源需要10000积分(如需开发票,请勿充值!)
    邮箱/手机:
    温馨提示:
    如需开发票,请勿充值!快捷下载时,用户名和密码都是您填写的邮箱或者手机号,方便查询和重复下载(系统自动生成)。
    如需开发票,请勿充值!如填写123,账号就是123,密码也是123。
    支付方式: 支付宝扫码支付    微信扫码支付   
    验证码:   换一换

    加入VIP,交流精品资源
     
    账号:
    密码:
    验证码:   换一换
      忘记密码?
        
    友情提示
    2、PDF文件下载后,可能会被浏览器默认打开,此种情况可以点击浏览器菜单,保存网页到桌面,就可以正常下载了。
    3、本站不支持迅雷下载,请使用电脑自带的IE浏览器,或者360浏览器、谷歌浏览器下载即可。
    4、本站资源下载后的文档和图纸-无水印,预览文档经过压缩,下载后原文更清晰。
    5、试题试卷类文档,如果标题没有明确说明有答案则都视为没有答案,请知晓。

    DIN EN 16521-2014 Cosmetics - Analytical methods - GC MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection German version .pdf

    1、July 2014 Translation by DIN-Sprachendienst.English price group 10No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 7

    2、1.100.70!%7?“2202898www.din.deDDIN EN 16521Cosmetics Analytical methods GC/MS method for the identification and assay of 12 phthalates incosmetic samples ready for analytical injection;English version EN 16521:2014,English translation of DIN EN 16521:2014-07Kosmetische Mittel Analysenmethoden GC/MS-

    3、Methode fr die Identifizierung und die Quantifizierung von 12 Phthalaten in zurdirekten Injektion geeigneten Proben kosmetischer Mittel;Englische Fassung EN 16521:2014,Englische bersetzung von DIN EN 16521:2014-07Cosmtiques Mthodes analytiques Mthode CG-SM pour lidentification et lanalyse de 12 phta

    4、lates dans des chantillons deproduits cosmtiques prts tre injects dans un systme analytique;Version anglaise EN 16521:2014,Traduction anglaise de DIN EN 16521:2014-07www.beuth.deDocument comprises 15 pagesIn case of doubt, the German-language original shall be considered authoritative.06.14 DIN EN 1

    5、6521:2014-07 2 A comma is used as the decimal marker. National foreword This document (EN 16521:2014) has been prepared by Technical Committee CEN/TC 392 “Cosmetics” (Secretariat: AFNOR, France). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwir

    6、tschaftliche Produkte (Food and Agricultural Products Standards Committee), Working Committee NA 057-07-01 AA Kosmetische Mittel. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16521 May 2014 ICS 71.100.70 English Version Cosmetics - Analytical methods - GC/MS method for the identification and

    7、 assay of 12 phthalates in cosmetic samples ready for analytical injection Cosmtiques - Mthodes analytiques - Mthode CG-SM pour lidentification et lanalyse de 12 phtalates dans des chantillons de produits cosmtiques prts tre injects dans un systme analytique Kosmetische Mittel - Analysenmethoden - G

    8、C/MS-Methode fr 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 con

    9、ditions 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 exis

    10、ts 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 sta

    11、ndards 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, S

    12、lovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reser

    13、ved worldwide for CEN national Members. Ref. No. EN 16521:2014 EEN 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 Det

    14、ection .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 DIN EN 16521:2014-07 EN 16521:2014 (

    15、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

    16、 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 su

    17、ch 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 Mace

    18、donia, 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. DIN EN 16521:2014-07 EN 16521:2014 (E) 4 Introduction Phthalates are

    19、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 mol

    20、ecular 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

    21、 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 Este

    22、rs 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

    23、(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

    24、. 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 m film thickness using a temperature gradient. Phthalate quantification i

    25、s 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. DIN EN 16521:2014-07 EN 16521:2014 (E) 5 1 Scope This European Standard describes a GC/MS method for the assay of 12 phthalat

    26、es, 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 aft

    27、er 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 Phthal

    28、ates CAS ManufacturerbQuality DBP a(dibutyl phthalate) 84742 ALDRICH 97,0 % DEHP a(diethylhexyl phthalate) 117817 ALDRICH 99,8 % BBP a(butylbenzyl phthalate) 85687 ALDRICH 97,0 % DMEP a(di(2-methoxyethyl) phthalate) 117828 ALDRICH 97,0 % DnPP a(di-n-pentyl phthalate) 131180 CIL CLUZEAU 99,0 % DiPP a

    29、(diisopentyl phthalate) 605505 CIL CLUZEAU 95,0 % DPP a(n-pentyl isopentyl phthalate) 84777060 CIL CLUZEAU 95,0 %* DiBP a(diisobutyl phthalate) 84695 ACROS 98,0 % DCHP (dicyclohexyl phthalate) 84617 ALDRICH 98,0 % DEP (diethyl phthalate) 84662 ACROS 98,0 % DMP (dimethyl phthalate) 131113 ACROS 98,0

    30、% DnOP (di-n-octyl phthalate) 117840 ALDRICH 98,0 % aRegulated phthalates. bThis 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, D

    31、nPP 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 g/ml. 1) This is an example of a suitable product available commercially. This information is given for the convenie

    32、nce of users of this document and does not constitute an endorsement by CEN of this product. DIN EN 16521:2014-07 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 calibr

    33、ation mark with ethanol. This stock solution is daily prepared. 2.5 Phthalates stock solution, c = 500 g/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.

    34、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 an

    35、d SM-2 at 1 000 g/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 mixin

    36、g equal volumes of both standard solutions (c = 500 g/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 fi

    37、lled with ethanol (2.2) up to the calibration mark (c = 50 g/ml). From this intermediate solution (S1), at least 5 calibration solutions are prepared by dilution in ethanol (2.2) after the addition of 100 l of the internal standard stock solution (SM-ISTD). Phthalates concentrations on these calibra

    38、tion solutions ranges from 0,25 g/ml to 5,0 g/ml with an ISTD concentration fixed at 10,0 g/ml. These calibration solutions are prepared extemporaneously and injected. If cosmetic samples (perfume) are directly prepared in a 1,5 ml GC vial, according to 4.2, the preparation of calibration solutions

    39、have to be adapted: Calibration solutions, ranging from 0,25 g/ml to 5,0 g/ml, are prepared without internal standard and 10 l of the internal standard stock solution (SM-ISTD) are added to 1,0 ml of each calibration solution directly in a 1,5 ml GC vial. These calibration solutions are prepared ext

    40、emporaneously. Vials are shaken and the solution injected. 3 Apparatus and equipment 3.1 Standard laboratory equipment. 3.2 Gas chromatography/mass spectrometry apparatus. 3.3 Gas chromatography/FID (for standard purity). 3.4 Analytical separation column. The following parameters have proved useful:

    41、 GC column, low bleeding phase: 5 %-Phenyl-95 %-dimethylpolysiloxane, 30 m 0,25 mm (i. d.) 0,25 m or equivalent material. 4 Procedure 4.1 Standard purity The purity of each standard and the internal standard and the respective percentages for geometrical isomers (n-pentyl isopentyl phthalate - DPP)

    42、shall be determined by GC-FID for further calculations. DIN EN 16521:2014-07 EN 16521:2014 (E) 7 4.2 Sample preparation 1,0 g of the cosmetic sample ready for analytical injection is transferred into a 10,0 ml volumetric flask and filled with ethanol (2.2) up to the calibration mark after the additi

    43、on of 100 l of the internal standard stock solution (SM-ISTD). This solution is injected. In case of excessive concentration of phthalates, an appropriate previous dilution of the sample is performed. The limit of quantification using this sample preparation was set at 5 ppm. An alternative sample p

    44、reparation consists to prepare the cosmetic sample directly in a 1,5 ml GC vial. 10 l of the internal standard stock solution (SM-ISTD) are added to 1,0 ml of cosmetic samples (perfume). Vials are shaken and the solution injected. The limit of quantification obtained using this sample preparation wa

    45、s set at 0,5 ppm. Calibration solutions are prepared according to 2.6. 4.3 Gas chromatography (GC) measurement conditions When using the apparatus (3.2) and column (3.4), the following conditions have shown to be useful: Table 2 GC/MS programme Apparatus Gas chromatography with mass selective detect

    46、or (GC/MS) Autosampler Column GC column, low bleeding phase: 5 %-Phenyl-95 %-dimethylpolysiloxane, 30 m 0,25 mm 0,25 m (or equivalent) Oven programme Ramp Temperature Time 100 C 0 min 30 C/min 200 C 0 min 3 C/min 260 C 0 min 30 C/min 320 C 5 min Injector T 300 C Interface T 250 C Source T 230 C Inje

    47、ction time 30 min Gas / flow rate He/1 ml/min Injection port split/splitless Injection parameters : 1 l/Constant pressure, Split 1/20 Detection mode Quadrupole Ionisation mode EI (70 eV) Mass detection (Full/SIM) Identification: full-scan (m/z 40 to 350) Quantification: SIM using 3 specific ions Int

    48、ernal standard 4,4-Dibromodiphenyl Calibration 0,25 g/ml to 5,0 g/ml Solvent used Ethanol (injection) DIN EN 16521:2014-07 EN 16521:2014 (E) 8 Examples of chromatogram, obtained using the GC/MS programme described in Table 2, are given in Annex A (Figure A.1). 4.4 Detection 4.4.1 General The detection and quantitative determination can be performed by evaluating the mass traces of each phthalate. Relative Retention (RR), m/z ions used for qua


    注意事项

    本文(DIN EN 16521-2014 Cosmetics - Analytical methods - GC MS method for the identification and assay of 12 phthalates in cosmetic samples ready for analytical injection German version .pdf)为本站会员(testyield361)主动上传,麦多课文档分享仅提供信息存储空间,仅对用户上传内容的表现方式做保护处理,对上载内容本身不做任何修改或编辑。 若此文所含内容侵犯了您的版权或隐私,请立即通知麦多课文档分享(点击联系客服),我们立即给予删除!




    关于我们 - 网站声明 - 网站地图 - 资源地图 - 友情链接 - 网站客服 - 联系我们

    copyright@ 2008-2019 麦多课文库(www.mydoc123.com)网站版权所有
    备案/许可证编号:苏ICP备17064731号-1 

    收起
    展开