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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 67.180.10 Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Unc
2、ontrolled Copy, (c) BSI BS EN 1377:1997 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
3、 the work on this standard: Committee reference AW/-/3 Draft for comment 94/501925 DC ISBN 0 580 27123 4 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 bodie
4、s 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 Amendments issued since publication Amd. No.DateComments Licensed Copy: sh
5、effieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 1377:1997 BSI 09-1999i Contents Page Committees responsibleInside front cover National forewordii Foreword2 Text of EN 13773 List of referencesInside back cover Licensed Copy: sheffieldun sheffieldun, na,
6、 Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 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 EN 1377:1996 Foodstuffs Determination of acesulfame K in table top sweetener prepa
7、rations 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. ISO 5725:1986, to which informative reference is made in the text, has been superseded by ISO 57
8、25-1:1994, 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
9、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 practi
10、ce 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. Cross-references P
11、ublication referred toCorresponding British Standard EN ISO 3696:1995BS 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, the EN title page, pages 2 to 6, an inside back
12、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. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EU
13、ROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1377 September 1996 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 Spectr
14、ometric method Produits alimentaires Dosage de lacsulfame K dans les dulcorants de table Mthode spectromtrique Lebensmittel Bestimmung von Acesulfam-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/
15、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 a
16、ny 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.
17、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 Comit Europen de Normalisation E
18、uropisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyright reserved to CEN members Ref. No. EN 1377:1996 E Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 1377:1996 BSI 09-1999 2 Foreword This Eu
19、ropean 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
20、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, Ital
21、y, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Contents Page Foreword2 1Scope3 2Normative references3 3Principle3 4Reagents3 5Apparatus and equipment3 6Procedure3 7Expression of results4 8Precision4 9Test report4 Annex A (informative) Figure5 Annex B
22、 (informative) Precision data6 Annex C (informative) Bibliography6 Figure A.1 Absorption spectrum of an acesulfame K standard solution in water5 Table B.16 Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 1377:1996 BSI 09-19993 1 Scope Thi
23、s 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. 2 Normative references This European Standard incorporates by dated or undated ref
24、erence, 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 incorpo
25、rated 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. 3 Principle Preparation of the sample test solution by dissolving table top sweetener preparation i
26、n water. Photometric determination of the acesulfame K content at the absorption maximum of about 227 nm. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and water of at least grade 3 as defined in EN ISO 3696. 4.1 Acesulfame K standard subst
27、ance, with a known content of at least 99 % in dry matter. NOTEFor further information on identification and purity, see 2. 4.2 Acesulfame K stock solution, (C4H4NO4SK) 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
28、volumetric flask, and dilute to the mark with water. 4.3 Acesulfame K standard solution, (C4H4NO4SK) 8 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. NOTEAdditional solutions with concentrations within the linear range
29、may be prepared for the calibration graph. 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 of 1 cm. 6 Procedure 6.1 Determination of ave
30、rage 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. NOTEFor 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 swe
31、etener 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 necessar
32、y, 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 quart
33、z 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 solutio
34、n 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 ca
35、se, the method is not applicable. 1) is the mass concentration. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 1377:1996 4 BSI 09-1999 Verify the applicability by determining the absorptions 12 nm above and 12 nm below the wavelength of
36、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. 7 Expression of results 7.1 Ca
37、lculate the mass fraction, w1, of acesulfame K, in milligrams per kilogram, using the following equation: Where: 7.2 Calculate the mass fraction, w2 of acesulfame K, in milligrams per tablet, using the following equation: where: If the calculation is based on a calibration graph, an alternative calc
38、ulative 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 precision of the method according to ISO 5725:1986 3 are summarized in Annex B. The values derived from the inter-laboratory test
39、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 t
40、he repeatability limit r in not more than 5 % 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 reproducibi
41、lity limit R in not more than 5 % 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 least the following data: all information necessary for the identification of the sample; a reference to this European Stand
42、ard 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
43、the results. (1) A2is the absorption of the sample test solution (6.3.2); A1is the absorption of the acesulfame K standard solution (6.3.1); m0is the initial sample mass (6.2) in milligrams; m1is the mass of the acesulfame K standard substance in 500 ml standard solution (4.3) in milligrams (here: 4
44、,0 mg); Fis the dilution factor (here: 100). (2) m2is the average tablet mass (6.1), in milligrams; A2, F, m1, A1, m0see equation (1). Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 1377:1996 BSI 09-19995 Annex A (informative) Figure Fig
45、ure A.1 Absorption spectrum of an acesulfame K standard solution in water Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:44:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 1377:1996 6 BSI 09-1999 Annex B (informative) Precision data In accordance with ISO 5725:1986 3, the following param
46、eters 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 Annex C (informative) Bibliography 1 Untersuchung von Lebensmitteln: Bestimmung des Acesulfam-K-Gehal
47、tes in acesulfam-K-haltigen Sstoff-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 Lebensmitte
48、ln, Tabakerzeugnissen, kosmetischen Mitteln und Bedarfsgegensnden/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) Loseblattaus
49、gabe, Stand Mai 1994. Bd. 1. (Loose-leaf edition of 1994-05. Vol. I.) Berlin, Kln: 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. SampleCommercially available acesulfame tablets Year of inter-laboratory test1986 Number of laboratories8 Number of samples1 Number of laborato