EN ISO 24444-2010 en Cosmetics - Sun protection test methods - In vivo determination of the sun protection factor (SPF)《化妆品 防晒试验方法 防晒因子(SPF)的体内测定》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 24444:2010Cosmetics Sun protectiontest methods In vivodetermination of the sunprotection factor (SPF) (ISO24444:2010)BS EN ISO 24444:2010 BRITISH STANDARDNational forew

2、ordThis British Standard is the UK implementation of EN ISO24444:2010.The UK participation in its preparation was entrusted to TechnicalCommittee CW/217, Cosmetics.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to in

3、clude all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 61111 7ICS 71.100.70Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy

4、 and Strategy Committee on 31 December 2010.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD 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 (SP

5、F) (ISO 24444:2010) Cosmtiques - Mthodes dessai de protection solaire - Dtermination in vivo du facteur de protection solaire (FPS) (ISO 24444:2010) Kosmetik - Untersuchungsverfahren fr Sonnenschutzmittel - In-vivo- Bestimmung des LSF (Lichtschutzfaktors) (ISO 24444:2010) This European Standard was

6、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 lists and bibliographical references concerning such nationa

7、l 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

8、 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, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

9、 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 NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels

10、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: EBS EN ISO 24444:2010EN ISO 24444:2010 (E) 3 Foreword This document (EN ISO 24444:2010) has been prepared by Technical Committee ISO/TC 217 “Cosmetics“ in collabo

11、ration 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 standard, either by publication of an identical text or by endorsement, at the latest by May 2011, and conflicting national standards shall b

12、e 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 and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulatio

13、ns, 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

14、Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 24444:2010 has been approved by CEN as a EN ISO 24444:2010 without any modification. BS EN ISO 24444:2010ISO 24444:2010(E) ISO 2010 All rights res

15、erved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Terms and definitions .1 3 General principle .2 4 Test subjects3 4.1 Selection of the test subjects.3 4.2 Number of test subjects3 4.3 Test area.4 5 Apparatus and materials 4 5.1 Source of ultraviolet radiation .4 5.2 Reference sunscreen f

16、ormulations .5 6 Procedure.6 6.1 Main steps 6 6.2 Test conditions6 6.3 Position of the test subjects 6 6.4 Procedure for product application 6 6.5 Procedure for UV exposure8 6.6 Product removal 9 6.7 Procedure for MED assessment 9 7 Calculation of the sun protection factor and statistics.10 7.1 Calc

17、ulation of the individual SPF (SPFi).10 7.2 Calculation of product SPF 10 7.3 Statistical criterion 10 7.4 Validation of the test .10 8 Test report11 Annex A (normative) Selection criteria for the test subjects .12 Annex B (normative) Definition of the UV solar simulator output.15 Annex C (normative

18、) SPF reference sunscreen formulations .23 Annex D (normative) Calculations and statistics 32 Annex E (informative) Colorimetric determination of skin colour typing and prediction of the minimal erythemal dose (MED) without UV exposure.38 Bibliography45 BS EN ISO 24444:2010ISO 24444:2010(E) iv ISO 2

19、010 All rights reservedForeword 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 through ISO technical committees. Each member body interested in

20、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 collaborates closely with the International Electrotechnical Commissi

21、on (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical c

22、ommittees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall n

23、ot be held responsible for identifying any or all such patent rights. ISO 24444 was prepared by Technical Committee ISO/TC 217, Cosmetics. BS EN ISO 24444:2010ISO 24444:2010(E) ISO 2010 All rights reserved vIntroduction The level of sun protection provided by sunscreen products has traditionally bee

24、n estimated using the sun protection factor or SPF test, which uses the erythemal 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 volunt

25、eers. It uses ultraviolet radiation usually from an artificial source. Different 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 i

26、s therefore necessary to get the same SPF value for a single product whatever the country in which it is tested. BS EN ISO 24444:2010BS EN ISO 24444:2010INTERNATIONAL STANDARD ISO 24444:2010(E) ISO 2010 All rights reserved 1Cosmetics Sun protection test methods In vivo determination of the sun prote

27、ction factor (SPF) 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 component able to absorb, reflect or scatter ultraviolet (UV) rays

28、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 the purposes of this document, the following terms and definit

29、ions 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 the range of 320 nm to 400 nm NOTE UVA II = 320 nm to 340 nm; U

30、VA 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 skin 2.4 minimal erythemal dose MED lowest dose of ultraviolet

31、 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 BS EN ISO 24444:2010ISO 24444:2010(E) 2 ISO 2010 All rights reserved2.4.1 MEDu MED on unprotected skin 2.4.2 MEDp MED on prod

32、uct 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(unprotectedskin) MEDuNOTE SPFi is expressed to one decimal

33、 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 the waist 2.8 test site site where a product i

34、s 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 method that utilizes a xenon arc lamp solar

35、 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 section of each subjects skin is exposed to

36、 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 validation of the procedure. To determine the sun p

37、rotection 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 evaluator. BS EN ISO 24444:2010ISO 24444:2010(E) I

38、SO 2010 All rights reserved 3The 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 protection factor (SPFi)

39、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 in the test. 4 Test subj

40、ects 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 have an ITA value 28 by c

41、olorimetric 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 subject at risk and that the

42、 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 included in the SPF test panel

43、. 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 two months have elapsed and

44、 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 subjects The minimum numb

45、er 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 number of test subjects used

46、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 the related protocol. BS EN

47、 ISO 24444:2010ISO 24444:2010(E) 4 ISO 2010 All rights reservedIn 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 subjects

48、 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 from a

49、 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 chosen 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 shoul