SIST EN 14333-1:2005
(Main)Non fatty foods - Determination of benzimidazole fungicides carbendazim, thiabendazole and benomyl (as carbendazim) - Part 1: HPLC method with solid phase extraction clean up
Non fatty foods - Determination of benzimidazole fungicides carbendazim, thiabendazole and benomyl (as carbendazim) - Part 1: HPLC method with solid phase extraction clean up
This draft European Standard specifies a high performance liquid chromatographic method for the determination of the benzimidazole fungicides carbendazim and thiabendazole in fruits and vegetables.
When benomyl is present, it is completely degraded to carbendazim and is also determined as carbendazim. Thiophanate-methyl is not determined with the method.
The method has been validated for carbendazim and thiabendazole in an interlaboratory test with homogenates of apples and oranges.
Fettarme Lebensmittel - Bestimmung der Benzimidazol-Fungizide Carbendazim, Thiabendazol und Benomyl (als Carbendazim) - Teil 1: HPLC-Vefahren mit Reinigung durch Festphasenextraktion
Diese Europäische Norm legt ein hochleistungs-flüssigchromatographisches Verfahren zur Bestimmung der Benzimidazol-Fungizide Carbendazim und Thiabendazol in Obst und Gemüse fest.
Wenn Benomyl anwesend ist, wird es vollständig zu Carbendazim abgebaut und ebenfalls als Carbendazim bestimmt. Thiophanat-methyl wird mit dem Verfahren nicht bestimmt.
Das Verfahren ist für Carbendazim und Thiabendazol durch einen Ringversuch mit Homogenaten von Äpfeln und Orangen validiert worden.
Aliments non gras - Détermination des benzimidazoles antifongiques : le carbendazime, le thiabendazole et le bénomyl en tant que carbendazime - Partie 1: Méthode CLHP avec purification par extraction en phase solide
Le présent projet de Norme européenne décrit une méthode de chromatographie en phase liquide a haute performance pour la détermination du carbendazime et du thiabendazole, benzimidazoles antifongiques, dans les fruits et les légumes.
Si du bénomyl est présent, celui-ci est completement dégradé en carbendazime et dosé comme du carbendazime. Le thiophanate-méthyle n'est pas dosé par cette méthode.
La présente méthode a été validée pour le carbendazime et le thiabendazole lors d'un essai interlaboratoires réalisé a l'aide de broyats d'oranges et de pommes.
Nemastna živila - Določevanje benzimidazolnih fungicidov: karbendazim, tiabendazol in benomil (kot karbendazim) - 1. del: Metoda HPLC s čiščenjem z ekstrakcijo na trdni fazi
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.D]LPFettarme Lebensmittel - Bestimmung der Benzimidazol-Fungizide Carbendazim, Thiabendazol und Benomyl (als Carbendazim) - Teil 1: HPLC-Vefahren mit Reinigung durch FestphasenextraktionAliments non gras - Détermination des benzimidazoles antifongiques : le carbendazime, le thiabendazole et le bénomyl en tant que carbendazime - Partie 1: Méthode CLHP avec purification par extraction en phase solideNon fatty foods - Determination of benzimidazole fungicides carbendazim, thiabendazole and benomyl (as carbendazim) - Part 1: HPLC method with solid phase extraction clean up67.080.01Sadje, zelenjava in njuni proizvodi na splošnoFruits, vegetables and derived products in general67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 14333-1:2004SIST EN 14333-1:2005en01-januar-2005SIST EN 14333-1:2005SLOVENSKI
STANDARD
SIST EN 14333-1:2005
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14333-1October 2004ICS 67.080.01 English versionNon fatty foods - Determination of benzimidazole fungicidescarbendazim, thiabendazole and benomyl (as carbendazim) -Part 1: HPLC method with solid phase extraction clean upAliments non gras - Détermination des benzimidazolesantifongiques : le carbendazime, le thiabendazole et lebénomyl en tant que carbendazime - Partie 1: MéthodeCLHP avec purification par extraction en phase solideFettarme Lebensmittel - Bestimmung der Benzimidazol-Fungizide Carbendazim, Thiabendazol und Benomyl (alsCarbendazim) - Teil 1: HPLC-Vefahren mit Reinigung durchFestphasenextraktionThis European Standard was approved by CEN on 29 July 2004.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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 translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14333-1:2004: ESIST EN 14333-1:2005
EN 14333-1:2004 (E) 2 Contents Page Foreword.3 1 Scope.4 2 Principle.4 3 Reagents.4 4 Apparatus.5 5 Procedure.6 6 Calculation.7 7 Confirmatory tests.7 8 Precision.8 9 Test report.9 Annex A (informative)
Precision data.10 Bibliography.12
SIST EN 14333-1:2005
EN 14333-1:2004 (E) 3 Foreword This document (EN 14333-1:2004) 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 April 2005, and conflicting national standards shall be withdrawn at the latest by April 2005.
EN 14333 consists of the following parts, under the general title Non fatty foods – Determination of benzimidazole fungicides carbendazim, thiabendazole and benomyl (as carbendazim): Part 1: HPLC method with solid phase extraction clean up; Part 2: HPLC method with gel permeation chromatography clean up; Part 3: HPLC method with liquid/liquid-partition clean up. WARNING — The use of this standard may involve hazardous materials, operations and equipment. This standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. SIST EN 14333-1:2005
EN 14333-1:2004 (E) 4 1 Scope This document specifies a high performance liquid chromatographic method for the determination of the benzimidazole fungicides carbendazim and thiabendazole in fruits and vegetables.
When benomyl is present, it is completely degraded to carbendazim and is also determined as carbendazim. Thiophanate-methyl is not determined with the method. The method has been validated for carbendazim and thiabendazole in an interlaboratory test with homogenates of apples and oranges.
2 Principle The sample is homogenized with acetone, dichloromethane and light petroleum and the homogenate is centrifuged to yield two layers of the supernatant. An aliquot portion of the upper layer is evaporated to dryness and the residue is dissolved in methanol containing benzimidazole as the internal standard. The solution is cleaned up by solid phase extraction (SPE) using a cartridge packed with diol-bonded silica. In the cartridge eluate, carbendazim and thiabendazole are determined by reversed-phase high performance liquid chromatography (HPLC) with UV or UV and fluorescence detectors.
3 Reagents 3.1 General Unless otherwise specified, use reagents of recognized analytical grade, preferably for HPLC and pesticide residue analysis, and only distilled or demineralized water. 3.2 Safety aspects associated with reagents Vapours from some volatile solvents are toxic. Several of these solvents are readily absorbed through skin. Use an effective fume hood to remove vapours of these solvents as they are set free. Carbendazim and thiabendazole are toxic; avoid contact with skin and eyes. 3.3 Acetone 3.4 Dichloromethane 3.5 Light petroleum, boiling range 40 °C to 60 °C 3.6 Methanol 3.7 Sodium hydroxide solution, mass concentration
(NaOH) = 4,0 g/100 ml
3.8 Ortho-Phosphoric acid, at least
(H3PO4) = 85 g/100 g
3.9 Phosphoric acid solution: To a 100 ml volumetric flask, transfer 0,6 ml ortho-phosphoric acid (3.8) and dilute to the mark with water. SIST EN 14333-1:2005
EN 14333-1:2004 (E) 5 3.10 SPE eluting mixture: Phosphoric acid solution (3.9) / methanol (3.6) 1 + 1 (V/V) 3.11 Phosphate buffer solution (pH 7): In a 500 ml volumetric flask, dissolve 1,76 g of potassium dihydrogen phosphate and 3,63 g of disodium hydrogen phosphate in water and dilute to the mark with water. 3.12 Mobile phase for HPLC: Methanol (3.6) / phosphate buffer solution (3.11) 7 + 3 (V/V). Prior to use, filter the mixture with suction through a membrane filter (4.9). 3.13 Carbendazim stock solution,
(carbendazim) = 10 mg/100 ml in methanol (3.6) 3.14 Thiabendazole stock solution,
(thiabendazole) = 10 mg/100 ml in methanol (3.6)
3.15 Benzimidazole stock solution,
(benzimidazole) = 10 mg/100 ml in methanol (3.6) 3.16 Internal standard solution,
(benzimidazole) = 0,50 µg/ml
In a 100 ml volumetric flask, dilute 500 µl of the benzimidazole stock solution (3.15) to the mark with methanol (3.6). 3.17 Standard solution,
(carbendazim) = 0,25 µg/ml,
(thiabendazole) = 0,25 µg/ml,
(benzimidazole) = 0,50 µg/ml Transfer 250 µl of carbendazim stock solution (3.13), 250 µl of thiabendazole stock solution (3.14) and 500 µl of benzimidazole stock solution (3.15) to a 100 ml volumetric flask and dilute to the mark with methanol (3.6) / phosphate buffer solution (3.11) 1 + 1 (V/V). 4 Apparatus 4.1 General Usual laboratory equipment and in particular the following: 4.2 Food chopper 4.3 Homogenizer or high speed blender 4.4 Centrifuge, provided with polytetrafluoroethylene tubes of capacity 250 ml, and capable of producing a rotational speed of at least 4000 min-1 4.5 Water bath, capable of being maintained at 60 °C 4.6 SPE cartridges, packed with 500 mg of the diol-bonded silica Bond Elut 2OH1), 40 µm irregular particles NOTE Several other brands have given unacceptable low recoveries, which is why the brand in this application is critical. 4.7 Device for eluting SPE cartridges (4.6), with suction NOTE Apparatus for automated SPE elution is commercially available. 4.8 High performance liquid chromatograph, equipped with SIST EN 14333-1:2005
EN 14333-1:2004 (E) 6 4.8.1 Pumping system, an injection valve for
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