1、BRITISH STANDARD BS EN 1377:1997 Foodstuffs Determination of acesulfame K in table top sweetener preparations Spectrometric method The European Standard EN 1377:1996 has the status of a British Standard ICS 67.180.10BSEN 1377:1997 This British Standard, having been prepared under the directionof the
2、 Consumer Products and Services Sector Board, was published under theauthority of the Standards Board and comes into effect on 15May1997 BSI 09-1999 The following BSI references relate to the work on this standard: Committee reference AW/-/3 Draft for comment 94/501925 DC ISBN 0 580 27123 4 Committe
3、es responsible for this British Standard The preparation of this British Standard was entrusted to Technical Panel AW/-/3, Food analysis Horizontal methods, upon which the following bodies were represented: Association of Public Analysts Food and Drink Federation Institute of Food Science and Techno
4、logy Laboratory of the Government Chemist Ministry of Agriculture, Fisheries and Food Royal Society of Chemistry Amendments issued since publication Amd. No. Date CommentsBSEN 1377:1997 BSI 09-1999 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 Text of EN 1
5、377 3 List of references Inside back coverBSEN 1377:1997 ii BSI 09-1999 National foreword This British Standard has been prepared by Technical Panel AW/-/3 and is the English language version of EN1377:1996 Foodstuffs Determination of acesulfame K in table top sweetener preparations Spectrometric me
6、thod, published by the European Committee for Standardization (CEN). EN1377 was produced as a result of international discussions in which the United Kingdom took an active part. ISO 5725:1986, to which informative reference is made in the text, has been superseded by ISO5725-1:1994, ISO5725-2:1994,
7、 ISO5725-3:1994, ISO5725-4:1994 and ISO5725-6:1994 which are identical with BS ISO5725 Accuracy (trueness and precision) of measurement methods and results, BSISO5725-1:1994 General principles and definitions, BS ISO5725-2:1994 Basic method for the determination of repeatability and reproducibility
8、of a standard measurement method, BS ISO5725-3:1994 Intermediate measures of the precision of a standard measurement method, BS ISO5725-4:1994 Basic method for the determination of the trueness of a standard measurement method, and BS ISO5725-6:1994 Use in practice of accuracy values. A British Stan
9、dard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-references Publication referred to Corresponding
10、British Standard EN ISO 3696:1995 BS EN ISO 3696:1995 Water for analytical laboratory use. Specification and test methods Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theEN title page, pages 2 to 6, an inside back cover and a back cover. This standar
11、d has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1377 September 1996 ICS 67.180.10 Descriptors: Food products, intense sweeteners, chemical an
12、alysis, determination of content, spectrometric analysis English version Foodstuffs Determination of acesulfame K in table top sweetener preparations Spectrometric method Produits alimentaires Dosage de lacsulfame K dans les dulcorants de table Mthode spectromtrique Lebensmittel Bestimmung von Acesu
13、lfam-K in Tafelsen Spektralphotometrisches Verfahren This European Standard was approved by CEN on 1996-06-09. 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 alte
14、ration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by trans
15、lation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembour
16、g, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyright reserved to CEN members Ref. No. EN 1377:1
17、996 EEN 1377:1996 BSI 09-1999 2 Foreword This European Standard has been prepared by the Technical Committee CEN/TC 275, Food analysis Horizontal methods, the Secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an ide
18、ntical text or by endorsement, at the latest by March1997, and conflicting national standards shall be withdrawn at the latest by March1997. According to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, F
19、rance, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Contents Page Foreword 2 1 Scope 3 2 Normative references 3 3 Principle 3 4 Reagents 3 5 Apparatus and equipment 3 6 Procedure 3 7 Expression of results 4 8
20、Precision 4 9 Test report 4 Annex A (informative) Figure 5 Annex B (informative) Precision data 6 Annex C (informative) Bibliography 6 Figure A.1 Absorption spectrum of an acesulfame K standard solution in water 5 Table B.1 6EN 1377:1996 BSI 09-1999 3 1 Scope This European Standard specifies a spect
21、rometric method for the determination of acesulfame K in solid table top sweetener preparations containing it. An inter-laboratory test has been carried out on sweetener tablets 1. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publica
22、tions. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision.
23、 For undated references the latest edition of the publication referred to applies. EN ISO 3696, Water for analytical laboratory use Specification and test methods. 3 Principle Preparation of the sample test solution by dissolving table top sweetener preparation in water. Photometric determination of
24、 the acesulfame K content at the absorption maximum of about227nm. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and water of at least grade3 as defined in EN ISO3696. 4.1 Acesulfame K standard substance, with a known content of at least99%
25、 in dry matter. NOTEFor further information on identification and purity, see2. 4.2 Acesulfame K stock solution, (C 4 H 4 NO 4 SK) 0,8g/l 1) Dissolve about400,0mg of the acesulfame K standard substance (4.1) weighed to the nearest0,1mg, in water in a500ml volumetric flask, and dilute to the mark wit
26、h water. 4.3 Acesulfame K standard solution, (C 4 H 4 NO 4 SK) 8 mg/l Pipette5,00ml of the acesulfame K stock solution(4.2) into a500ml volumetric flask and dilute to the mark with water. NOTEAdditional solutions with concentrations within the linear range may be prepared for the calibration graph.
27、5 Apparatus and equipment Usual laboratory apparatus and, in particular, the following. 5.1 Spectrometer, suitable for measurements in the ultraviolet (UV) range. 5.2 Quartz cuvettes, with an optical path length of1cm. 6 Procedure 6.1 Determination of average tablet mass Determine the mass of at lea
28、st20 sweetener tablets to the nearest0,1mg and calculate the average mass (m 2 ) of one tablet. NOTEFor improved accuracy the use of100 tablets is recommended. 6.2 Preparation of the sample test solution Dissolve an amount of finely ground table top sweetener preparation (m 0 ), equivalent to about4
29、00mg of acesulfame K or corresponding to20times the average mass of a tablet (6.1), transfer to a500ml volumetric flask with water, dissolve it in water and dilute to the mark with water. Allow any undissolved constituents to settle and, if necessary, filter the solution, discarding the first100ml o
30、f the filtrate. Then pipette5,00ml of the solution into a500ml volumetric flask and dilute to the mark with water. 6.3 Determination 6.3.1 Measure the absorption spectrum of the standard acesulfame K solution between200nm and 280 nm in quartz cuvettes (5.2) with water as reference and determine the
31、absorption (A 1 ) at the wavelength of the absorption maximum (about227nm). Check the linearity range with a series of solutions of suitable concentrations (calibration graph). 6.3.2 Measure the absorption spectrum of the sample test solution as described in6.3.1 and determine the absorption (A 2 )
32、at the absorption maximum as determined in6.3.1. If the shape of the absorption curve obtained for the sample test solution (6.2) differs from that of the standard solution, it is probable that an interfering substance is present. In this case, the method is not applicable. 1) is the mass concentrat
33、ion.EN 1377:1996 4 BSI 09-1999 Verify the applicability by determining the absorptions12nm above and12nm below the wavelength of the absorption maximum (about227nm). Absorption ratios between these values and the maximum absorption shall not differ from those obtained when using the acesulfame K sta
34、ndard solution (4.3). An example for an absorption spectrum of acesulfame K is given inAnnex A. 7 Expression of results 7.1 Calculate the mass fraction, w 1 , of acesulfame K, in milligrams per kilogram, using the following equation: Where: 7.2 Calculate the mass fraction, w 2of acesulfame K, in mil
35、ligrams per tablet, using the following equation: where: If the calculation is based on a calibration graph, an alternative calculative evaluation using the regression graph may be used. Report the result after rounding to one decimal place. 8 Precision Details of the inter-laboratory test of the pr
36、ecision of the method according to ISO5725:1986 3 are summarized inAnnex B. The values derived from the inter-laboratory test may not be applicable to analyte concentration ranges and matrices other than given inAnnex B. 8.1 Repeatability The absolute difference between two single test results found
37、 on identical test material by one operator using the same apparatus within the shortest feasible time interval will exceed the repeatability limit r in not more than5% of the cases. The value is: r = 3,2 mg/100 mg for commercially available acesulfame K tablets. 8.2 Reproducibility The absolute dif
38、ference between two single test results on identical test material reported by two laboratories will exceed the reproducibility limit R in not more than5% of the cases. The value is: R = 3,7 mg/100 mg for commercially available acesulfame K tablets. 9 Test report The test report shall contain at lea
39、st the following data: all information necessary for the identification of the sample; a reference to this European Standard or to the method used; the results and the units in which the results have been expressed; if the repeatability of the method has been verified; any particular points observed
40、 in the course of the test; any operations not specified in the method or regarded as optional which might have affected the results. (1) A 2 is the absorption of the sample test solution (6.3.2); A 1 is the absorption of the acesulfame K standard solution (6.3.1); m 0 is the initial sample mass (6.
41、2) in milligrams; m 1 is the mass of the acesulfame K standard substance in 500 ml standard solution (4.3) in milligrams (here: 4,0 mg); F is the dilution factor (here: 100). (2) m 2 is the average tablet mass(6.1), in milligrams; A 2 , F, m 1 , A 1 , m 0 see equation (1).EN 1377:1996 BSI 09-1999 5
42、Annex A (informative) Figure Figure A.1 Absorption spectrum of an acesulfame K standard solution in waterEN 1377:1996 6 BSI 09-1999 Annex B (informative) Precision data In accordance with ISO5725:1986 3, the following parameters have been defined in an inter-laboratory test. The test was conducted b
43、y the Max von Pettenkofer Institute of the Federal Health Office, Food Chemistry Department, Berlin, Germany 1. Table B.1 Annex C (informative) Bibliography 1 Untersuchung von Lebensmitteln: Bestimmung des Acesulfam-K-Gehaltes in acesulfam-K-haltigen Sstoff-Tabletten L 57.22.99-3, Mai 1989 (Food Ana
44、lysis: Determination of acesulfame K content in sweetener tablets containing it L 57.22.99-3, 1989-05) In: Amtliche Sammlung von Untersuchungsverfahren nach 35 LMBG: Verfahren zur Probenahme und Untersuchung von Lebensmitteln, Tabakerzeugnissen, kosmetischen Mitteln und Bedarfsgegensnden/Bundesgesun
45、dheitsamt (In: Collection of official methods under article35 of the German Federal Foods Act; Methods of sampling and analysis of foods, tobacco products, cosmetics and commodity goods, Federal Health Office) Loseblattausgabe, Stand Mai 1994. Bd.1.(Loose-leaf edition of 1994-05. Vol. I.) Berlin, Kl
46、n: Beuth Verlag GmbH. 2 FAO Food and Nutrition Paper28 of the Joint FAO/WHO Expert Committee on Food Additives, April1980. 3 ISO 5725:1986 Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. Sample Commercially available
47、acesulfame tablets Year of inter-laboratory test 1986 Number of laboratories 8 Number of samples 1 Number of laboratories retained after eliminating outliers 7 Number of outliers (laboratories) 1 Number of accepted results 38 Mean value 98,0 mg/100 mg Repeatability standard deviation s r 1,1 mg/100
48、mg Repeatability relative standard deviation RSD r 1,2 % Repeatability limit r 3,2 mg/100 mg Reproducibility standard deviation s R 1,3 mg/100 mg Reproducibility relative standard deviation RSD R 1,3 % Reproducibility limit R 3,7 mg/100 mg xBSEN 1377:1997 BSI 09-1999 List of references See national
49、foreword.BS EN 1377:1997 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions BritishStandards are updated by amendment or revision. Users of BritishStandards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to im
