00971287 PDF 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[.]
BRITISH STANDARD 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 67.180.10 BS EN 1377:1997 BS EN 1377:1997 Committees 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 Technology Laboratory of the Government Chemist Ministry of Agriculture, Fisheries and Food Royal Society of Chemistry This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was published under the authority of the Standards Board and comes into effect on 15 May 1997 © 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 580 27123 Amendments issued since publication Amd No Date Comments BS EN 1377:1997 Contents Committees responsible National foreword Foreword Text of EN 1377 List of references © BSI 09-1999 Page Inside front cover ii Inside back cover i BS EN 1377:1997 National foreword This British Standard has been prepared by Technical Panel AW/-/3 and is the English language version of EN 1377:1996 Foodstuffs — Determination of acesulfame K in table top sweetener preparations — Spectrometric method, published by the European Committee for Standardization (CEN) EN 1377 was produced as a result of international discussions in which the United Kingdom took an active part Cross-references Publication referred to Corresponding British Standard EN ISO 3696:1995 BS EN ISO 3696:1995 Water for analytical laboratory use Specification and test methods ISO 5725:1986, to which informative reference is made in the text, has been superseded by ISO 5725-1:1994, ISO 5725-2:1994, ISO 5725-3:1994, ISO 5725-4:1994 and ISO 5725-6:1994 which are identical with BS ISO 5725 Accuracy (trueness and precision) of measurement methods and results, BS ISO 5725-1:1994 General principles and definitions, BS ISO 5725-2:1994 Basic method for the determination of repeatability and reproducibility of a standard measurement method, BS ISO 5725-3:1994 Intermediate measures of the precision of a standard measurement method, BS ISO 5725-4:1994 Basic method for the determination of the trueness of a standard measurement method, and BS ISO 5725-6:1994 Use in practice of accuracy values A British Standard 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 Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages to 6, an inside back cover and a back cover This standard 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 ii © BSI 09-1999 EUROPEAN STANDARD EN 1377 NORME EUROPÉENNE September 1996 EUROPÄISCHE NORM ICS 67.180.10 Descriptors: Food products, intense sweeteners, chemical analysis, determination of content, spectrometric analysis English version Foodstuffs — Determination of acesulfame K in table top sweetener preparations — Spectrometric method Produits alimentaires — Dosage de l’acésulfame K dans les édulcorants de table — Méthode spectrométrique Lebensmittel — Bestimmung von Acesulfam-K in Tafelsüßen — 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 alteration 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 translation 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, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom CEN European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels © 1996 Copyright reserved to CEN members Ref No EN 1377:1996 E EN 1377:1996 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 identical text or by endorsement, at the latest by March 1997, and conflicting national standards shall be withdrawn at the latest by March 1997 According to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom Contents Foreword Scope Normative references Principle Reagents Apparatus and equipment Procedure Expression of results Precision Test report Annex A (informative) Figure Annex B (informative) Precision data Annex C (informative) Bibliography Figure A.1 — Absorption spectrum of an acesulfame K standard solution in water Table B.1 Page 3 3 3 4 6 © BSI 09-1999 EN 1377:1996 Scope Apparatus and equipment This European Standard specifies a spectrometric 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] 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 of cm Normative references This European Standard incorporates by dated or undated reference, provisions from other publications 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 For undated references the latest edition of the publication referred to applies EN ISO 3696, Water for analytical laboratory use — Specification and test methods Principle Preparation of the sample test solution by dissolving table top sweetener preparation in water Photometric determination of the acesulfame K content at the absorption maximum of about 227 nm Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and water of at least grade as defined in EN ISO 3696 4.1 Acesulfame K standard substance, with a known content of at least 99 % in dry matter NOTE For further information on identification and purity, see [2] 4.2 Acesulfame K stock solution, Ô(C4H4NO4SK) ë 0,8 g/l1) Dissolve about 400,0 mg of the acesulfame K standard substance (4.1) weighed to the nearest 0,1 mg, in water in a 500 ml volumetric flask, and dilute to the mark with water 4.3 Acesulfame K standard solution, Ô(C4H4NO4SK) ë mg/l Pipette 5,00 ml of the acesulfame K stock solution (4.2) into a 500 ml volumetric flask and dilute to the mark with water Procedure 6.1 Determination of average tablet mass Determine the mass of at least 20 sweetener tablets to the nearest 0,1 mg and calculate the average mass (m2) of one tablet NOTE For improved accuracy the use of 100 tablets is recommended 6.2 Preparation of the sample test solution Dissolve an amount of finely ground table top sweetener preparation (m0), equivalent to about 400 mg of acesulfame K or corresponding to 20 times the average mass of a tablet (6.1), transfer to a 500 ml 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 first 100 ml of the filtrate Then pipette 5,00 ml of the solution into a 500 ml 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 between 200 nm and 280 nm in quartz cuvettes (5.2) with water as reference and determine the absorption (A1) at the wavelength of the absorption maximum (about 227 nm) 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 in 6.3.1 and determine the absorption (A2) at the absorption maximum as determined in 6.3.1 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 NOTE Additional solutions with concentrations within the linear range may be prepared for the calibration graph 1) Ơ is the mass concentration © BSI 09-1999 EN 1377:1996 Verify the applicability by determining the absorptions 12 nm above and 12 nm below the wavelength of the absorption maximum (about 227 nm) Absorption ratios between these values and the maximum absorption shall not differ from those obtained when using the acesulfame K standard solution (4.3) An example for an absorption spectrum of acesulfame K is given in Annex A Expression of results 7.1 Calculate the mass fraction, w1, of acesulfame K, in milligrams per kilogram, using the following equation: (1) Where: A2 A1 m0 m1 F is the absorption of the sample test solution (6.3.2); is the absorption of the acesulfame K standard solution (6.3.1); is the initial sample mass (6.2) in milligrams; is the mass of the acesulfame K standard substance in 500 ml standard solution (4.3) in milligrams (here: 4,0 mg); is the dilution factor (here: 100) 7.2 Calculate the mass fraction, w2 of acesulfame K, in milligrams per tablet, using the following equation: (2) where: m2 A2, F, m1, A1, m0 is the average tablet mass (6.1), in milligrams; see equation (1) 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 Precision Details of the inter-laboratory test of the precision of the method according to ISO 5725:1986 [3] are summarized in Annex B The values derived from the inter-laboratory test may not be applicable to analyte concentration ranges and matrices other than given in Annex B 8.1 Repeatability The absolute difference between two single test results found 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 than % of the cases The value is: r = 3,2 mg/100 mg for commercially available acesulfame K tablets 8.2 Reproducibility The absolute difference between two single test results on identical test material reported by two laboratories will exceed the reproducibility limit R in not more than % of the cases The value is: R = 3,7 mg/100 mg for commercially available acesulfame K tablets Test report The test report shall contain at least 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 in the course of the test; — any operations not specified in the method or regarded as optional which might have affected the results © BSI 09-1999 EN 1377:1996 Annex A (informative) Figure Figure A.1 — Absorption spectrum of an acesulfame K standard solution in water © BSI 09-1999 EN 1377:1996 Annex B (informative) Precision data In accordance with ISO 5725:1986 [3], the following parameters have been defined in an inter-laboratory test The test was conducted by the Max von Pettenkofer Institute of the Federal Health Office, Food Chemistry Department, Berlin, Germany [1] Table B.1 Sample Year of inter-laboratory test Number of laboratories Number of samples Number of laboratories retained after eliminating outliers Number of outliers (laboratories) Number of accepted results Commercially available acesulfame tablets Mean value x 1986 38 98,0 mg/100 mg Repeatability standard deviation sr 1,1 mg/100 mg Repeatability relative standard deviation RSDr 1,2 % Repeatability limit r Reproducibility standard deviation sR 3,2 mg/100 mg 1,3 mg/100 mg Reproducibility relative standard deviation RSDR 1,3 % Reproducibility limit R 3,7 mg/100 mg Annex C (informative) Bibliography [1] Untersuchung von Lebensmitteln: Bestimmung des Acesulfam-K-Gehaltes in acesulfam-K-haltigen Süßstoff-Tabletten L 57.22.99-3, Mai 1989 (Food Analysis: 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 Bedarfsgegensänden/Bundesgesundheitsamt (In: Collection of official methods under article 35 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 (Loose-leaf edition of 1994-05 Vol I.) Berlin, Köln: Beuth Verlag GmbH [2] FAO Food and Nutrition Paper 28 of the Joint FAO/WHO Expert Committee on Food Additives, April 1980 [3] ISO 5725:1986 Precision of test methods — Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests © BSI 09-1999 BS EN 1377:1997 List of references See national foreword © BSI 09-1999 BS EN 1377:1997 BSI — British Standards Institution BSI is the independent national body responsible for preparing British Standards It presents the UK view on standards in Europe and at the international level It is incorporated by Royal Charter Revisions British Standards are updated by amendment or revision Users of British Standards should make sure that they possess the latest amendments or editions It is the constant aim of BSI to improve the quality of our products and services We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover Tel: 020 8996 9000 Fax: 020 8996 7400 BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services Tel: 020 8996 9001 Fax: 020 8996 7001 In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been published as British Standards, unless otherwise requested Information on standards BSI provides a wide range of information on national, European and international standards through its Library and its Technical Help to Exporters Service Various BSI electronic information services are also available which give details on all its products and services Contact the Information Centre Tel: 020 8996 7111 Fax: 020 8996 7048 Subscribing members of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards For details of these and other benefits contact Membership Administration Tel: 020 8996 7002 Fax: 020 8996 7001 Copyright Copyright subsists in all BSI publications BSI also holds the copyright, in the UK, of the publications of the internationalstandardization bodies Except as permitted under the Copyright, Designs and Patents Act 1988 no extract may be reproduced, stored in a retrieval system or transmitted in any form or by any means – electronic, photocopying, recording or otherwise – without prior written permission from BSI This does not preclude the free use, in the course of implementing the standard, of necessary details such as symbols, and size, type or grade designations If these details are to be used for any other purpose than implementation then the prior written permission of BSI must be obtained BSI 389 Chiswick High Road London W4 4AL If permission is granted, the terms may include royalty payments or a licensing agreement Details and advice can be obtained from the Copyright Manager Tel: 020 8996 7070