1、 STD-BSI BS EN 1379-ENGL 1997 m Lb24bb9 Ob3333b 87T m BRITISH STANDARD Foodstuffs - Determination of cyclamate and saccharin in liquid table top sweetener preparations - Method by high performance liquid chromatography The European Standard EN 1379 : 1996 has the status of a British standard ICs 67.
2、180.10 BS EN 1379 : 1997 -o n-m U- NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGH LAW u m STD=BSI BS EN L379-ENGL 1997 lb2Lib09 Ob33337 72b = BS EN 1379 : 1997 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Pane
3、l AW/-B, Food analysis - Horizontad methods, upon which the following bodies were represented: Associaion of Public Analysts Food and Drink Federation institute of Food Science and Technology Laboratory of the Government Chemist Mirustsy of Agriculture, Fisheries and Food Royal Society of Chemistry
4、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 O BSI 1997 Amendments issued since publication ID* I Te* The following BSI references rela
5、te to the work on this standard Committee reference Awl43 Draft for comment 94601927 DC ISBN O 580 27126 O STD-BSI BS EN 1379-ENGL 1777 W Lb2VbbS b33338 bb2 m BS EN 1379 : 1997 Contents page Committees responsible Inside front cover National foreword ii Foreword 2 Text of EN 1379 3 i BS EN 1379 : 19
6、97 National foreword This British Standard has been prepared by Technid Panel AW/-B and is the English language version of EN 1379 : 1996 Foodstufls -Determination of cz/clamate and saccharin in liquid W bp sweeten.erprt.pamtions -Method by high peomnce liquid chrvrnuiagraphy, published by the Europ
7、ean Committee for Smdardization (CEN). EN 1379 was produced as a result of internaional discussions in which the United Kingdom took an active part. Cross-references Publication referred to EN IS0 3696 : 1995 Corresponding British Standard BS EN IS0 3696 : 1995 Water fw analytical ZuZ)omton/ use. Sp
8、e LD isthelossinmassondqing,inoh 4.6.4 Sorbic acid toclc SOlUt.ion, p (CH3(CH) A2 is the peak area or peak height for sodium cyclamate, saccharin or sorbic acid obtained with the standard test solution, in units of ama or length; VI is the total volume of sample test solution (see 6.2), in miliditre
9、s (here: 100 mi); V2 is the total volume of standard test solution (see 4.7), in miilitres (here: 100 mi); m is the mass of standard substances of sodium cyclamate and saccharin, in grams, or of sorbic acid, in V2, in milligrams, respectiveiy, comected for the loss in mass on drymg; F is the ciiluti
10、on factor (here: 10); is the initiai amount of sample, in milliiitres. Report the result for sodium cyclamate or cyclamic acid after rounding to one decimal place, for sodium saccharin or saccharin as free imide after roundmg to two decimal places and for sorbic acid without any decimal places, acco
11、rding to current legisation. 7.3 When determining sodium cyclamate only peak areas can be used for evaluation since the peak is not symmetrical. 8 Precision Details of the inter-laboratory test of the precision of the method according to IS0 5725 : 1986 3 are summarized in annex B. The dues derived
12、from the inter-iaboraory test may not be applicable to analyte concentration ranges and mahices other than given in annex B. O BSI 1997 STDeBSI BS EN L379-ENGL L997 = Lb24bb9 Ob333i.15 AT2 Page 6 EN 1379 : 1996 8.1 Repeatability The absolute difference between two single test results found on identi
13、cal test material by one operator using the same apparatw within the shortest feasible time inkrva will exceed the repeatability limit r in not more than 5% of the cases. The values are: sodium cyclamate r = 0,69 g/100 mi for liquid table top Saccharin r = 0,03 g/100 mi for liquid table top sorbic a
14、cid r = 2 mg/100 mi for liquid table top sweetener preparation sweetener preparation sweetener preparation 8.2 Reproducibility The absolute difference between two single test results on identicai test material reported by two laboratories wiii exceed the reproducibility limit R in not more than 5 %
15、of the cases. The values are: 9 %st report The test report shall contain at least the following dak - ali 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 resuits have been express - if
16、 the repeatabdiw 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. soium cyclamate R = 1,0 g/100 mi for liquid table top SacCharin sorbic acid sweete
17、ner preparation sweetener preparation sweetener preparation R = 0,O g/100 ml for liquid table top R = 8 mg/lOo ml for liquid table top O BSI 1997 STD*BSI BS EN 1377-ENGL 1997 lb24bb7 Ob3334b 739 Page 7 EN 1379 : 1996 Annex A (informative) Figures O1 4 30 C O .- CI L $ 2 O e 2 ,h 0 -e o (b o .- E 6 c
18、 6 min 10 Time Liquid table top sweetener preparation (dilution 1 + 199) separahg column Length Diameter Mobile phase Flow UV detection iqection volume (contents: sodium cyclamate 600 mu, saccharin 53 mg/i, sorbic acid 2,3 mg/i) Nucleosi 1206) C 18 4,6 mm 250 mm potassium dihydrogen orthophosphate s
19、olution (c = 0,0125 movI)/HPLC methanol (7030 VIV) + phosphoric acid H = 4,5) 1,7 nVmin 200 nm (1), 260 nm (2) and 265 nm (3) 20 4 Figure A.l. HPLC separation of a liquid table top sweetener preparation 1 Nucleosil 120 is a tradename of a product supplied by Macherey-Nagel, Diiren. This information
20、is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product named. Quivalent products may be used if they can be shown to lead to the same results. O BSI 1997 STD.BSI BS EN 1377-ENGL 1977 LbZi.lbb9 b33347 b75 Page 8 EN 1379 : 1996 Sam
21、ple Solvent Concentration Function Wavelength range 1 Sodium cylmate Mobile phase (see 4.4) 4g/l Absorption 200 nm to 300 nm 1 1 c lo O .- c L a O :o a O O Wavelength - Recognized maximum: 1: Wavelength = 202 nm Absorption = 1,588959 Figure A.2. Absorption spectrum of a sodium cyclamate standard sol
22、ution (in mobile phase as described in 4.4) O BSI 1997 Page 9 EN 1379 : 1996 Sample Solvent Concentration Function Sodium saccharin Mobile phase (see 4.4) Absorption 100 mg/i 1 2.6034 2,1061 I 1,6049 c O .- c Q L O D 1.1056 a O, O. 3 60634 - 200 210 220 230 240 250 260 270 280 290nm300 Wavelength -
23、Recognized maxima or minima: 1: Wavelength = 224 nm 2: Wavelength = 246 nm 3 Wavelength = 268 nm Absorption = 2,603378 Absorption = 0,550720 Absorption = 0,834274 Figure A.3. Absorption spectrum of a sodium saccharin standard solution (in mobile phase as described in 4.4) O BSI 1997 Page 10 EN 1379
24、: 1996 Year of inkr-labomtory test Number of laboratories Number of samples Number of laboratories retained after eliminating outliers Number of outliers (laboratories) Number of accepted results Annex B (informative) Precision data In accordance with IS0 5725 : 1986 3, the following parameters have
25、 been defined in an inter-laboratory test. The test was conducted by the Max von Petknkofer Institute of the Federal Health Office, Food Chemistry Department, Berlin, Germany l. sodium cyclamate 1989 8 1 6 2 30 hble B.l. SamDle I Lianid table to sweetener DreDarations Mean value X Repeaability stand
26、ard deviation s, Rewzdzibility relatsve standard deviation RSDr 12,02 g100 ml 0,24 g100 ml 2,05 % Repeatabiity limit r I 0,69 g/100 ml Reproducibility standard deviation SR Reproducibity relative standard deviation RSh 0,35 u100 ml 2,97 % Reproducibility limit R I 1,o dloo ml accharin 1989 8 1 7 1 3
27、5 1,06 g/100 ml 3,Ol g100 ml 1,01% 3,33 g/100 ml ),O3 g100 ml 1,70 % ),O8 d100 ml sorbic acid 1989 8 1 7 1 35 30 md100 ml 3,6 mg/100 ml 1,38 % 1 mg100 ml 3 mg100 ml 3,52 % 3 md100 ml Annex C (informative) Bibliography i Untersuchung von Lebensmitteln: Bestimmung des Natriumychmt, Smchrin und Sortnns
28、ure in IWsigbfe L 57.22.99-5, Dezember 1990 (Food Analysis: Determinution of the contents of sodium cyciamute, saccharin and sodric ac in liquid table top meeteneus L 57.22.94-5,19912) In: Amtliche Sammung von Unkrwhungahm nach 5 35 LMBG: Vyliirm zur Probenahme und Untersuchung wm IebensrnitMn, 5%.h
29、kmwken, hsmetkch Mitteln und Bedarjsgegenst4n.d Buncesgsu7n Methods of sampling and amysis of foods, tobacco pmducts, cosmetics and commodity goods/Federal Health Onice) Loseblattausgabe, Stand Mai 1994.M 1 (Loose-leaf edition of 1994-05 Vol. I.) Berlin, Kln: Beuth Verhg GmbH. 2 FA0 Food and Nutriti
30、on Paper 17 of the Joint FAOWHO Expert Committee on Food Additives, Aprii 1980. 3 Is0 5725 : 1986Preckion of test methods - Determinution of repeatability and reproducibity for a standan test method by interiubomtom/ tests. O BSI 1997 STD-BSI BS EN 1379-ENGL 1997 W 1bZibbS Ob33350 LbT BS EN 1379 : 1
31、997 List of references See national foreword. O BSI 1997 STD*BSI BS EN L377-ENGL 1777 LbZqbbS Ob33351 OTb BS EN 1379 : 1997 BSI 389 Chiswick High Road London w4 4AL BSI - British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the U
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