DIN EN ISO 24444-2011 Cosmetics - Sun protection test methods - In vivo determination of the sun protection factor (SPF) (ISO 24444 2010) German version EN ISO 24444 2010《化妆品 防晒试验方.pdf

1、March 2011 Translation by DIN-Sprachendienst.English price group 20No 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

2、71.100.70!$n:%“1752302www.din.deDDIN EN ISO 24444Cosmetics Sun protection test methods English translation of DIN EN ISO 24444:2011-03Kosmetik Untersuchungsverfahren fr Sonnenschutzmittel Englische bersetzung von DIN EN ISO 24444:2011-03Cosmtiques Mthodes dssai de protection solaire Dtermination du

3、facteur de protection solaire (FPS) (ISO 24444:2010)Traduction anglaise de DIN EN ISO 24444:2011-03www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.51In vivoIn-vivoin vivodetermination of the sun protection factor (SPF) (ISO 24444:2

4、010)-Bestimmung des Sonnenschutzfaktors (SSF) (ISO 24444:2010)03.11 DIN EN ISO 24444:2011-03 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 217 “Cosmetics” (Secretariat: ISIRI, Iran) in collaboration with Technical Committee C

5、EN/TC 392 “Cosmetics” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Working Committee NA 057-07-01 AA Kosmetische Mittel. EUROPEAN ST

6、ANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 24444 November 2010 ICS 71.100.70 English Version Cosmetics Sun protection test methods In vivo determination of the sun protection factor (SPF) (ISO 24444:2010) Cosmtiques Mthodes dessai de protection solaire Dtermination in vivo du facteur de protectio

7、n solaire (FPS) (ISO 24444:2010) This European Standard was approved by CEN on 26 May 2010. 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

8、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 un

9、der 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, France

10、, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR N

11、ORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 24444:2010: EKosmetik Untersuchungsverfahren fr Sonnenschutzmittel In-vivo-Bestimmung des Sonnenschutzfaktors (SSF

12、) (ISO 24444:2010) Contents Page Foreword3 Introduction .4 1 Scope 5 2 Terms and definitions .5 3 General principle6 4 Test subjects7 4.1 Selection of the test subjects .7 4.2 Number of test subjects7 4.3 Test area .8 5 Apparatus and materials.8 5.1 Source of ultraviolet radiation8 5.2 Reference sun

13、screen formulations9 6 Procedure .10 6.1 Main steps 10 6.2 Test conditions 10 6.3 Position of the test subjects.10 6.4 Procedure for product application.10 6.5 Procedure for UV exposure 12 6.6 Product removal.13 6.7 Procedure for MED assessment.13 7 Calculation of the sun protection factor and stati

14、stics .14 7.1 Calculation of the individual SPF (SPFi) .14 7.2 Calculation of product SPF.14 7.3 Statistical criterion.14 7.4 Validation of the test .14 8 Test report 15 Annex A (normative) Selection criteria for the test subjects16 Annex B (normative) Definition of the UV solar simulator output .19

15、 Annex C (normative) SPF reference sunscreen formulations27 Annex D (normative) Calculations and statistics 36 Annex E (informative) Colorimetric determination of skin colour typing and prediction of the minimal erythemal dose (MED) without UV exposure .42 Bibliography 49 DIN EN ISO 24444:2011-03 EN

16、 ISO 24444:2010 (E) 2 Foreword This document (EN ISO 24444:2010) has been prepared by Technical Committee ISO/TC 217 “Cosmetics” in collaboration with Technical Committee CEN/TC 392 “Cosmetics” the secretariat of which is held by NEN. This European Standard shall be given the status of a national st

17、andard, either by publication of an identical text or by endorsement, at the latest by May 2011, and conflicting national standards shall be withdrawn at the latest by May 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN

18、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, C

19、zech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 24444:2

20、010 has been approved by CEN as a EN ISO 24444:2010 without any modification. DIN EN ISO 24444:2011-03 EN ISO 24444:2010 (E) 3 Introduction The level of sun protection provided by sunscreen products has traditionally been estimated using the sun protection factor or SPF test, which uses the erythema

21、l response of the skin to ultraviolet (UV) radiation. The SPF is a ratio calculated from the energies required to induce a minimum erythemal response with and without sunscreen product applied to the skin of human volunteers. It uses ultraviolet radiation usually from an artificial source. Different

22、 standard methods are available and described in the technical report ISO/TR 263694. These standards are similar by some parameters but different by others. Differences can lead to discrepancy of results. Harmonization is therefore necessary to get the same SPF value for a single product whatever th

23、e country in which it is tested. DIN EN ISO 24444:2011-03 EN ISO 24444:2010 (E) 4 1 Scope This International Standard specifies a method for the in vivo determination of the sun protection factor (SPF) of sunscreen products. This International standard is applicable to products that contain any comp

24、onent able to absorb, reflect or scatter ultraviolet (UV) rays and which are intended to be placed in contact with human skin. It provides a basis for the evaluation of sunscreen products for the protection of human skin against erythema induced by solar ultraviolet rays. 2 Terms and definitions For

25、 the purposes of this document, the following terms and definitions apply. 2.1 ultraviolet radiation UVR electromagnetic radiation in the range of 290 nm to 400 nm 2.1.1 ultraviolet B UVB electromagnetic radiation in the range of 290 nm to 320 nm 2.1.2 ultraviolet A UVA electromagnetic radiation in

26、the range of 320 nm to 400 nm NOTE UVA II = 320 nm to 340 nm; UVA I = 340 nm to 400 nm. 2.2 erythema reddening of the skin caused by UV radiation 2.3 sunscreen products products containing any component able to absorb, reflect or scatter UV rays, which are intended to be placed in contact with human

27、 skin 2.4 minimal erythemal dose MED lowest dose of ultraviolet radiation (UVR) that produces the first perceptible unambiguous erythema with defined borders appearing over most of the field of UV exposure, 16 h to 24 h after UV exposure DIN EN ISO 24444:2011-03 EN ISO 24444:2010 (E) 5 2.4.1 MEDu ME

28、D on unprotected skin 2.4.2 MEDp MED on product protected skin 2.5 individual sun protection factor SPFi ratio of the minimal erythemal dose on product protected skin (MEDp) to the minimal erythemal dose on unprotected skin (MEDu) of the same subject: MED(protectedskin) MEDpSPFi= =MED(unprotectedski

29、n) MEDuNOTE SPFi is expressed to one decimal place (see 7.1). 2.6 sun protection factor of a product SPF arithmetic mean of all valid individual SPFi values obtained from all subjects in the test NOTE SPF is expressed to one decimal place (see 7.2). 2.7 test area back between the scapula line and th

30、e waist 2.8 test site site where a product is applied or the site used for the determination of the unprotected MED 2.9 exposure sub-sites skin exposed spots 2.10 individual typology angle ITA value characterizing the skin colour of the subject 3 General principle The SPF test method is a laboratory

31、 method that utilizes a xenon arc lamp solar simulator (or equivalent) of defined and known output to determine the protection provided by sunscreen products on human skin against erythema induced by solar ultraviolet rays. The test is restricted to the area of the back of selected human subjects. A

32、 section of each subjects skin is exposed to ultraviolet light without any protection and another (different) section is exposed after application of the sunscreen product under test. One further section is exposed after application of an SPF reference sunscreen formulation which is used for validat

33、ion of the procedure. To determine the sun protection factor, incremental series of delayed erythemal responses are induced on a number of small sub-sites on the skin. These responses are visually assessed for presence of redness 16 h to 24 h after UV radiation, by the judgment of a competent evalua

34、tor. DIN EN ISO 24444:2011-03 EN ISO 24444:2010 (E) 6 The minimal erythemal dose (MED) for unprotected skin (MEDu) and the MED obtained after application of a sunscreen product (i.e. the MED for product protected skin, MEDp) shall be determined on the same subject on the same day. An individual sun

35、protection factor (SPFi) for each subject tested is calculated as the ratio of individual MED on product protected skin divided by the individual MED on unprotected skin i.e. MEDp/MEDu. The sun protection factor for the product (SPF) is the arithmetic mean of all valid SPFi results from each subject

36、 in the test. 4 Test subjects 4.1 Selection of the test subjects 4.1.1 General For subject inclusion and non inclusion criteria, refer to Annex A. 4.1.2 Skin phototype of the test subjects Test subjects included in the SPF test shall be only phototypes I, II or III according to Fitzpatrick7or shall

37、have an ITA value 28 by colorimetric methods (see Annexes A and E) and be untanned on the test area. An SPF test should not contain subjects who are all of the same phototype. A competent scientist or technician should examine each subject to ensure that there is no condition which might put the sub

38、ject at risk and that the outcome of the test cannot be compromised by adverse skin conditions such as sun damage, pigmentation marks and previous history of abnormal response to the sun (see Annex A). 4.1.3 Age restriction Test subjects below the age of consent or older than 70 y shall not be inclu

39、ded in the SPF test panel. 4.1.4 Frequency of participation in tests Since a sufficient interval after a previous test is needed in order to allow for reversal of skin tanning resulting from that previous test, a test site that has been exposed to UV should not be used in a subsequent test before tw

40、o months have elapsed and the site is clear. 4.1.5 Ethics and consent All testing shall be done in accordance with the Declaration of Helsinki8and National Regulations regarding human studies, if any. Informed, written (signature) consent shall be obtained from all test subjects. 4.2 Number of test

41、subjects The minimum number of valid SPFi results shall be 10 and the maximum number of valid SPFi results shall be 20. In order to achieve between 10 and 20 valid results, a maximum of five individual invalid results may be excluded from the calculation of the mean SPF. Consequently the actual numb

42、er of test subjects used will fall between a minimum of 10 and a maximum of 25 subjects (i.e. a maximum of 20 valid results plus 5 rejected invalid results). Results may only be declared invalid and excluded from the calculation of the mean SPF according to 6.7.4 or because of non-compliance with th

43、e related protocol. DIN EN ISO 24444:2011-03 EN ISO 24444:2010 (E) 7 In order to determine the number of test subjects, the 95 % confidence interval (95 % CI) on the mean SPF shall be taken into account. A minimum of 10 subjects shall be tested. The test shall be considered valid for the first 10 su

44、bjects if the resulting range of the 95 % CI of the mean SPF is within 17 % of the mean SPF. If it is not within 17 % of the mean SPF, the number of subjects shall be increased stepwise from the minimum number of 10 until the 95 % CI statistical criterion is met (up to a maximum of 20 valid results

45、from a maximum of 25 subjects tested). If the statistical criterion has not been met after 20 valid results from a maximum of 25 subjects, then the test shall be rejected. For details on statistical definitions, sequential procedure and calculations, refer to Annex D. 4.3 Test area The back is the c

46、hosen anatomical region for the test area. The individual product test sites and the unprotected test site shall be delineated within the region between the scapula line and the waist. Skeletal protrusions and extreme areas of curvature should be avoided. 5 Apparatus and materials 5.1 Source of ultr

47、aviolet radiation 5.1.1 General The artificial light source used shall comply with the source spectral specifications as described in 5.1.2 and Annex B. A xenon arc solar simulator with appropriate filters is recommended. 5.1.2 Quality of ultraviolet radiation 5.1.2.1 The solar UV simulator shall em

48、it a continuous spectrum with no gaps or extreme peaks of emission in the UV region. The output from the solar UV simulator shall be stable, uniform across the whole output beam (particularly important for a single large-beam) and suitably filtered to create a spectral quality that complies with the

49、 required acceptance limits (see Table B.1). 5.1.2.2 To ensure that appropriate amounts of UVA radiation are included in the spectrum of the solar UV simulator, the total radiometric proportion of the UVA II (320 nm to 340 nm) irradiance of the simulator shall W 20 % of the total UV (290 nm to 400 nm) irradiance. Additionally, the UVA I region (340 nm to 400 nm) irradiance shall be W 60 % of the total UV irradiance. 5.1.2.3 The source spectral specification is described in terms of cumulative erythemal effectiveness by successive wave