SIST EN 16155:2012
(Main)Foodstuffs - Determination of sucralose - High performance liquid chromatographic method
Foodstuffs - Determination of sucralose - High performance liquid chromatographic method
This European Standard specifies a method for the determination of sucralose in foodstuffs by high performance liquid chromatography (HPLC) by means of elution from a reversed-phased (RP) column using aqueous methanol, followed by RI detection. This method has been validated in an interlaboratory study via the analysis of sucralose (from 83 mg/kg to 737 mg/kg) in spiked samples of ketchup, mayonnaise, biscuits, yoghurt, instant beverage powder and sweets. For further information on the validation results see Annex C.
Lebensmittel - Bestimmung von Sucralose - Hochleistungsflüssigchromatographisches Verfahren
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Sucralose in Lebensmitteln mit ochleistungsflüssigkeitschromatographie (HPLC) durch Elution von einer Umkehrphasensäule (RP-Säule) unter Verwendung von wässrigem Methanol und anschließender RI-Detektion fest. Das Verfahren wurde in einem Ringversuch durch Analyse von Sucralose (von 83 mg/kg bis 737 mg/kg) in aufgestockten Proben von Ketchup, Mayonnaise, Keksen, Joghurt, sofort löslichem Getränkepulver und Süßwaren (Komprimaten) validiert. Hinsichtlich weiterer Informationen zu den Validierungsergebnissen siehe Anhang C.
Produits alimentaires - Détermination du sucralose - Méthode par chromatographie liquide à haute performance
La présente Norme européenne spécifie une méthode de dosage du sucralose dans les produits alimentaires par chromatographie liquide à haute performance (CLHP), par élution sur une colonne en phase inverse (PI) en utilisant du méthanol aqueux, suivie d’une détection de l’indice de réfraction. Cette méthode a été validée lors d’une étude interlaboratoires via l’analyse du sucralose (de 83 mg/kg à 737 mg/kg) dans des échantillons dopés de ketchup, mayonnaise, biscuits, yaourt, poudre pour boisson instantanée et bonbons.
Pour de plus amples informations sur les résultats de validation, voir l’Annexe C.
Živila - Določevanje sukraloze - Tekočinska kromatografija visoke ločljivosti
Ta evropski standard določa metodo za določevanje sukraloze v živilih s tekočinsko kromatografijo visoke ločljivosti (HPLC) prek elucije iz reverzne fazne (RP) kolone z uporabo vodnega metanola in pozneje z določanjem lomnega količnika. Ta metoda je bila validirana z medlaboratorijsko raziskavo prek analize sukraloze (od 83 mg/kg do 737 mg/kg) v primešanih vzorcih kečapa, majoneze, piškotov, jogurta, instantne pijače v prahu in sladkarij. Za več informacij o rezultatih validacije glejte dodatek C.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Sucralose - Hochleistungsflüssigchromatographisches VerfahrenProduits alimentaires - Détermination du sucralose - Méthode par chromatographie liquide à haute performanceFoodstuffs - Determination of sucralose - High performance liquid chromatographic method67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 16155:2012SIST EN 16155:2012en,fr,de01-september-2012SIST EN 16155:2012SLOVENSKI
STANDARD
SIST EN 16155:2012
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16155
April 2012 ICS 67.050 English Version
Foodstuffs - Determination of sucralose - High performance liquid chromatographic method
Produits alimentaires - Dosage du sucralose - Méthode par chromatographie liquide à haute performance
Lebensmittel - Bestimmung von Sucralose - Hochleistungsflüssigchromatographisches Verfahren This European Standard was approved by CEN on 25 February 2012.
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 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 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, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
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Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16155:2012: ESIST EN 16155:2012
EN 16155:2012 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Principle .44Reagents .45Apparatus and equipment .56Procedure .66.1Sample preparation .66.2Preparation of the sample test solutions .66.2.1Soluble samples (e. g. hard candies and similar products) .66.2.2Incompletely soluble samples (e. g. pastries, chewing gum, yoghurt, ketchup, mayonnaise) .66.2.3Solid phase extraction .66.3High-performance liquid chromatography (HPLC) .66.4Identification .66.5Quantitative determination .77Calculation .78Precision .78.1General .78.2Repeatability .78.3Reproducibility .89Test report .8Annex A (informative)
Statistical data of the inter-laboratory trial .9Bibliography . 11 SIST EN 16155:2012
EN 16155:2012 (E) 3 Foreword This document (EN 16155:2012) has been prepared by 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 October 2012, and conflicting national standards shall be withdrawn at the latest by October 2012. 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 Regulations, 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16155:2012
EN 16155:2012 (E) 4 1 Scope This European Standard specifies a method for the determination of sucralose in foodstuffs by high performance liquid chromatography (HPLC) by means of elution from a reversed-phased (RP) column using aqueous methanol, followed by RI detection [1]. This method has been validated in an inter-laboratory study via the analysis of sucralose (from 83 mg/kg to 737 mg/kg) in spiked samples of ketchup, mayonnaise, biscuits, yoghurt, instant beverage powder and sweets. For further information on the validation results, see Annex A. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) 3 Principle Depending on their consistency, the samples are either dissolved in water or diluted with water and, if appropriate, they are filtered or clarified with modified Carrez solutions. Afterwards, they are extracted on a solid phase extraction column and eluted with a mixture of methanol/water. The sucralose content is determined by high-performance liquid chromatography (HPLC) by means of elution from a reversed-phased (RP) column using aqueous methanol, followed by RI (refractive index) detection. Alternatively, an ELSD (Evaporative Light Scattering Detector) may be used. Quantification is performed by applying the external standard method. The content of sucralose in foodstuffs means identifying the content of 1,6-dichloro-1,6-dideoxy-β-D-fructofuranosyl-4-chloro-4-deoxy-α-D-galactopyranoside, as determined in accordance with the method described in this document.
4 Reagents Use only reagents of recognized analytical grade and water complying with grade 1 of EN ISO 3696:1995, unless otherwise specified. Solvents shall be of the same quality used for HPLC analysis, unless otherwise specified. Commercially available solutions with equivalent properties to the reagents listed may be used.
4.1 Sucralose, (C12H19Cl3O8, MW: 397,63). 4.2 Potassium hexacyanoferrate(II), K4[Fe(CN)6] ⋅ 3H2O. 4.3 Zinc nitrate, Zn(NO3)2 ⋅ 6H2O. 4.4 Methanol for HPLC. 4.5 Stock solution (Suc ≈ 1 000 mg/l). Weigh approximately 100 mg of sucralose to the nearest 0,1 mg in a 100 ml volumetric flask; dissolve in a small amount of water and dilute to the calibration mark with water. Prepare the solution fresh every day. The water content and the purity of the standard substance shall be taken into consideration.
SIST EN 16155:2012
EN 16155:2012 (E) 5 4.6 Standard solutions (Suc = 20 mg/l to 100 mg/l). The concentrations of the standard solution given in the following are examples only and may be changed depending on the devices' sensitivity and the concentration range to be covered. Care shall be taken not to exceed the linear range of the detector system.
Prepare from the stock solution (4.5) at least five standard solutions by diluting in such a way that sucralose concentrations of e.g., 20 mg/l, 40 mg/l, 60 mg/l, 80 mg/l and 100 mg/l are obtained. Prepare these solutions fresh every day of the analysis. 4.7
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