EN 16158:2012
(Main)Animal feeding stuffs - Determination of semduramicin content - Liquid chromatographic method using a "tree" analytical approach
Animal feeding stuffs - Determination of semduramicin content - Liquid chromatographic method using a "tree" analytical approach
This European standard specifies a high-performance liquid chromatographic (HPLC) method for the determination of the semduramicin content at authorized level in animal feeding stuffs [2], using mass spectrometry detection or post-column derivatization and (UV)-VIS detection (hereinafter UV detection). This method is applicable to poultry feed. The limit of quantitation is 1,0 mg/kg when mass spectrometry is used for detection and 3,0 mg/kg when the detection is performed by UV with post-column derivatization. Lower limits of quantitation are achievable but this is to be validated by the user.
The method allows the discrimination of semduramicin from monensin, salinomycin, narasin, maduramicin and lasalocid.
Futtermittel - Bestimmung des Semduramicingehalts - Flüssigkeitschromatographisches Verfahren mit verzweigter analytischer Vorgehensweise
Diese Europäische Norm legt ein hochleistungsflüssigkeitschromatographisches (HPLC) Verfahren zur Bestimmung des Semduramicingehaltes bei einem zugelassenen Gehalt in Futtermitteln [2] mittels massen-spektrometrischer Detektion oder Nachsäulenderivatisierung und (UV) VIS-Detektion (nachstehend UV Detektion) fest. Das Verfahren gilt für Geflügelfutter. Bei der Anwendung von Massenspektrometrie zum Nachweis beträgt die Bestimmungsgrenze 1,0 mg/kg und beim Nachweis mittels UV mit Nachsäulenderivatisierung 3,0 mg/kg. Niedrigere Bestimmungsgrenzen sind erreichbar, das ist jedoch vom Anwender zu validieren.
Das Verfahren ermöglicht es, Semduramicin von Monensin, Salinomycin, Narasin, Maduramicin und Lasalocid zu unterscheiden.
Aliments pour animaux - Dosage de la semduramicine - Chromatographie liquide utilisant une approche analytique en arbre
La présente Norme européenne spécifie une méthode de dosage de la semduramicine au taux autorisé dans les aliments pour animaux, par chromatographie liquide haute performance (CLHP) [2] avec détection par spectrométrie de masse ou dérivation post-colonne et détection UV/VIS (désignée par détection UV ci-après). Cette méthode est applicable aux aliments pour volailles. La limite de quantification est de 1,0 mg/kg avec détection par spectrométrie de masse et de 3,0 mg/kg avec détection UV et dérivation post-colonne. Des limites de quantification inférieures peuvent être obtenues, à condition qu'elles soient validées par l'utilisateur.
La méthode permet de différencier la semduramicine du monensine, de la salinomycine, du narasine, de la maduramicine et du lasalocide.
Krma - Določevanje semduramicina - Metoda tekočinske kromatografije z "razvejanim" analitskim pristopom
Ta evropski standard določa metodo tekočinske kromatografije visoke ločljivosti (HPLC) za določevanje dovoljene vrednosti vsebnosti semduramicina v krmi [2] z masno spektrometrijo ali postkolonsko derivatizacijo in zaznavanjem (UV)-VIS (v nadaljnjem besedilu: zaznavanje UV). Ta metoda se uporablja za perutninsko krmo. Če se za zaznavanje uporablja masna spektrometrija, je meja kvantifikacije 1,0 mg/kg, če pa se zaznavanje izvaja z zaznavanjem UV s postkolonsko derivatizacijo, pa 3,0 mg/kg. Nižje meje kvantifikacije so dosegljive, vendar jih mora validirati uporabnik. Metoda omogoča razlikovanje semduramicina od monenzina, salinomicina, narazina, maduramicina in lasalocida.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Futtermittel - Bestimmung des Semduramicingehalts - Flüssigkeitschromatographisches Verfahren mit verzweigter analytischer VorgehensweiseAliments pour animaux - Dosage de la semduramicine - Chromatographie liquide utilisant une approche analytique en arbreAnimal feeding stuffs - Determination of semduramicin content - Liquid chromatographic method using a "tree" analytical approach65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN 16158:2012SIST EN 16158:2012en,fr,de01-april-2012SIST EN 16158:2012SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16158
February 2012 ICS 65.120 English Version
Animal feeding stuffs - Determination of semduramicin content -Liquid chromatographic method using a "tree" analytical approach
Aliments pour animaux - Dosage de la semduramicine - Chromatographie liquide utilisant une approche analytique en arbre
Futtermittel - Bestimmung des Semduramicingehalts - Flüssigkeitschromatographisches Verfahren mit verzweigter analytischer Vorgehensweise This European Standard was approved by CEN on 30 December 2011.
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.
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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 16158:2012: ESIST EN 16158:2012
Results of collaborative study . 17A.1Procedure . 17A.2Statistical analysis of results . 18A.3Example chromatogram . 22Bibliography . 25
4 Reagents Use only reagents of recognized analytical grade, unless otherwise specified.
4.1 LC-MS. 4.1.1 Water, HPLC grade, or equivalent (e.g. Milli-Q purified water). 4.1.2 Acetonitrile, HPLC gradient grade, minimum 99,9 % purity. 4.1.3 Methanol, HPLC grade or hypergrade LC-MS. 4.1.4 Ammonium formate, HPLC grade. 4.1.5 Mobile phase. 4.1.5.1 Ammonium formate solution, c = 20 mmol/l. Accurately weigh 1,25 g to the nearest 0,01 g of ammonium formate (4.1.4) into a 1 000 ml volumetric flask. Dissolve in water (4.1.1) and make up to 1 000 ml of volume with water. Prepare fresh solutions monthly. 4.1.5.2 HPLC mobile phase. SIST EN 16158:2012
4.2.4.2 Ammonium formate solution, c = 100 mmol/l at pH = 3. Accurately weigh 6,30 g to the nearest 0,01 g of ammonium formate (4.1.4) into a 1 000 ml volumetric flask (5.7). Dissolve in 900 ml water (4.1.1). Adjust the pH to 3,0 using formic acid (4.2.3) and make up to 1 000 ml with purified water. Prepare fresh monthly. 4.2.4.3 HPLC mobile phase (solvent blank). Mix methanol (4.1.3) and ammonium formate solution (4.2.4.2) in proportion of 90+10 (v+v). Filter under a vacuum using a solvent filtration system (5.11) and Nylon filters (5.13). 4.3 Reference standards LC-PCD-UV method. WARNING — Avoid inhalation of and exposure to the toxic standard materials and solutions thereof. Work in a fume-hood when handling the solvents and solutions. Wear safety glasses and protective clothing.
Declaration of purity is required for each lot of reference standard.
4.3.1 Semduramicin sodium standard, minimum 93 % purity expressed as semduramicin.
NOTE Available from Phibro Animal Health Corporation, Third Floor 65 Challenger Road Ridgefield Park, NJ 07660-2103 USA. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of the product named. Equivalent products may be used if they can be shown to lead to the same results. 4.4 Reference standards LC-MS method. In addition to the reference standard 4.3.1: 4.4.1 Nigericin sodium standard, minimum 98 % purity to be used as internal standard (I.S.). NOTE Available from Calbiochem, A Brand of EMD Biosciences, Inc. 10394 Pacific Center Court, San Diego, CA 92121 USA. This information is given for the convenience of users of this European Standard and does not constitute an SIST EN 16158:2012
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