EN 12014-4:2005

Foodstuffs - Determination of nitrate and/or nitrite content - Part 4: Ion-exchange chromatographic (IC) method for the determination of nitrate and nitrite content of meat products

This European Prestandard specifies an ion-exchange chromatographic method for the determination of the nitrate and nitrite contents of meat products having a nitrate content of 50 mg/kg to 300 mg/kg as nitrate ions and a nitrite content of approximately 40 mg/kg as nitrite ion. Note: Validation data obtained from interlaboratory studies show that this method may also be applied to the determination of nitrate in vegetables and baby food, see (1), (2). Furthermore, the method may be applied for the determination of nitrite in meat products having a nitrite content of greater than 40 mg/kg.

Lebensmittel - Bestimmung des Nitrat- und/oder Nitritgehaltes - Teil 4: Ionenchromatographisches Verfahren (IC) für die Bestimmung des Nitrat- und Nitritgehaltes in Fleischerzeugnissen

Diese Europäische Norm legt ein Ionenaustausch-chromatographisches Verfahren zur Bestimmung des Nitrit-
und Nitratgehaltes von Fleischerzeugnissen fest und wurde an verschiedenen Fleischerzeugnissen mit einem
Nitratgehalt von 50 mg/kg bis 300 mg/kg als Nitrat-Ion und einem Nitritgehalt von etwa 40 mg/kg als Nitrit-Ion
validiert.
ANMERKUNG Zuverlässigkeitsdaten aus Ringversuchen zeigen, dass dieses Verfahren auch für die Bestimmung von
Nitrat in Gemüse und Säuglingsnahrung angewendet werden kann, siehe [1], [2]. Des Weiteren darf das Verfahren für die
Bestimmung des Nitritgehaltes in Fleischerzeugnissen mit einem Nitritgehalt von mehr als 40 mg/kg angewendet werden.

Produits alimentaires - Détermination de la teneur en nitrates et/ou en nitrites - Partie 4 : Détermination par chromatographie ionique (CI) de la teneur en nitrates et en nitrites dans les produits carnés

Cette Norme européenne spécifie une méthode de détermination par chromatographie ionique de la teneur en
nitrates et en nitrites dans les produits carnés, et a été validée pour différents produits carnés pour une teneur
en nitrates comprise entre 50 mg/kg et 300 mg/kg, exprimée en ion nitrate et une teneur en nitrites d�environ
40 mg/kg, exprimée en ion nitrite.
NOTE Les données de validation issues des essais interlaboratoires montrent que cette méthode peut s'appliquer
également pour la détermination des nitrates dans les légumes et les aliments pour bébés [1], [2]. De plus, cette méthode
peut être utilisée pour la détermination des nitrites dans les produits carnés ayant une teneur en nitrites supérieure à
40 mg/kg.

Živila – Določevanje nitratov in/ali nitritov - 4. del: Metoda ionske izmenjalne kromatografije za določevanje nitratov in nitritov v mesnih proizvodih

General Information

• Status: Published
• Publication Date: 17-May-2005
• Withdrawal Date: 29-Nov-2005
• ICS: 67.120.10 - Meat and meat products
• Technical Committee: CEN/TC 275 - Food analysis - Horizontal methods
• Drafting Committee: CEN/TC 275/WG 7 - Nitrate, nitrite
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Completion Date: 04-Sep-2019
• Ref Project: SIST EN 12014-4:2005 - Foodstuffs - Determination of nitrate and/or nitrite content - Part 4: Ion-exchange chromatographic (IC) method for the determination of nitrate and nitrite content of meat products

Relations

• Replaces: ENV 12014-4:1998 - Foodstuffs - Determination of nitrate and/or nitrite content - Part 4: Ion-exchange chromatographic (IC) method for the determination of nitrate and nitrite content of meat products
• Effective Date: 22-Dec-2008

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.YRGLKLebensmittel - Bestimmung des Nitrat- und/oder Nitritgehaltes - Teil 4: Ionenchromatographisches Verfahren (IC) für die Bestimmung des Nitrat- und Nitritgehaltes in FleischerzeugnissenProduits alimentaires - Détermination de la teneur en nitrates et/ou en nitrites - Partie 4 : Détermination par chromatographie ionique (CI) de la teneur en nitrates et en nitrites dans les produits carnésFoodstuffs - Determination of nitrate and/or nitrite content - Part 4: Ion-exchange chromatographic (IC) method for the determination of nitrate and nitrite content of meat products67.120.10Meso in mesni proizvodiMeat and meat products67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 12014-4:2005SIST EN 12014-4:2005en01-september-2005SIST EN 12014-4:2005SLOVENSKI
STANDARDSIST ENV 12014-4:19991DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12014-4
May 2005 ICS 67.120.10 Supersedes ENV 12014-4:1998 English version
Foodstuffs - Determination of nitrate and/or nitrite content - Part 4: Ion-exchange chromatographic (IC) method for the determination of nitrate and nitrite content of meat products
Produits alimentaires - Détermination de la teneur en nitrates et/ou en nitrites - Partie 4: Détermination par chromatographie ionique (CI) de la teneur en nitrates et en nitrites dans les produits à base de viande
Lebensmittel - Bestimmung des Nitrat- und/oder Nitritgehaltes - Teil 4: Ionenchromatographisches Verfahren (IC) für die Bestimmung des Nitrat- und Nitritgehaltes in Fleischerzeugnissen This European Standard was approved by CEN on 1 April 2005.
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 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 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.
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 STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36
B-1050 Brussels © 2005 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12014-4:2005: ESIST EN 12014-4:2005

Example for an IC chromatogram of corned beef
(Sample from the interlaboratory test).10 Annex B (informative)
Precision data.11 Annex C (informative)
Further applicability.13 Bibliography.16
Dilute 15 ml of hydrochloric acid of 20 (HCl) = 1,18 g/ml in a 100 ml volumetric flask to the mark with water and mix. 4.7 Hydrochloric acid, c (HCl) ≈ 0,1 mol/l Dilute 5 ml of hydrochloric acid (4.6) in a 100 ml volumetric flask to the mark with water and mix.
1) c is the substance concentration SIST EN 12014-4:2005

NOTE Gluconic acid sometimes has a dark brown colour. In this case it is recommended to clarify it until a slight yellow colour is obtained. Generally two cartridges activated with methanol are necessary. 4.11 Lithium borate gluconate buffer solution To 500 ml of water in a 1000 ml volumetric flask add 34,00 g of boric acid (4.5) and 19,6 ml of gluconic acid solution (4.10). Dissolve completely in the solution 11,00 g of anhydrous lithium hydroxide or 19,26 g of lithium hydroxide monohydrate (4.4). Add 125 ml of glycerol (4.3), dilute to the mark with water and mix well. This solution is stable for 6 months if stored in a refrigerator at approximately 4 °C. 4.12 Mobile phase To 500 ml of water in a 1000 ml volumetric flask, add 17 ml of buffer solution (4.11) and 125 ml of acetonitrile (4.2). Dilute to the mark with water. Mix well. Adjust the pH to 6,5 ± 0,1 by adding hydrochloric acid (4.6 then 4.7). Filter through a membrane filter of pore size of approximately 0,22 µm (5.6). This solution is stable for not longer than one week and the pH value shall be checked every day before use. If the pH value falls outside the stated range, prepare a new solution.
2) This solution is commercially available. SIST EN 12014-4:2005

5.3 Magnetic stirrer (optional) 5.4 Fluted filter paper (nitrate/nitrite free), care is needed in the choice of filter paper as some can absorb nitrate. 5.5 Membrane filter, for aqueous and acetonitrile solutions, with a pore size of approximately 0,45 µm. 5.6 Membrane filter, for aqueous and acetonitrile solutions, with a pore size of approximately 0,22 µm. 5.7 Filter holder for membrane filter, with suitable syringe. 5.8 pH meter
5.9 Solid phase extraction column RP C18, with suitable syringe (optional). 5.10 IC apparatus, comprising the following 5.10.1 Isocratic high performance liquid chromatography unit, with a UV detector, capable of measuring at a wavelength of 205 nm and an evaluation unit (e.g an integrator with plotter). 5.10.2 Analytical separating column, Anion exchanger, 4,6 mm × 150 mm, packing material; polymethacrylate resin with a quarternary ammonium functional group, particle size of 10 µm, capacity (30 ± 3) µ eq/ml with a precolumn, e.g. 20 mm, having the same packing to protect the analytical column. 6 Procedure
6.1 Sample preparation Homogenize the laboratory sample with the appropriate equipment (5.2). Take care that the temperature of the sample material does not rise above 25 °C. If a mincer is used, pass the sample at least twice through the equipment. Weigh, to the nearest 10 mg, 10 g of the homogenized sample into e.g. a 150 ml wide neck conical flask (test portion).
6.2 Extraction and clarification
The analysis should be performed in a single working day. Add 50 ml of water at a temperature of 50 °C to 60 °C to the test portion in the wide neck flask. Mix thoroughly with the homogenizer (5.2). Rinse the homogenizer with water and add the washings to the flask. Quantitatively transfer this slurry into a 200 ml volumetric flask by rinsing the wide neck flask with water. Add 50 ml of acetonitrile (4.2). Mix gently. Allow to cool to room temperature. Dilute to the mark with water. SIST EN 12014-4:2005

6.4.1 IC operating conditions
If the column specified in 5.10.2 is used, it has been found satisfactory to adopt the following parameters. Mobile phase: as described in 4.12 UV: 205 nm Injection volume: 40 µl (minimum) Flow rate: 1 ml/min If other columns than the one described in 5.10.2 are used, adjust chromatographic conditions. 6.4.2 IC measurement
Inject the standard solutions (4.9) first and then the blank and the sample test solutions under the conditions as described in 6.4.1. One of the standard solutions should be injected every five sample test solutions when performing a series of analyses. If the peak obtained for the sample falls outside the range of the calibration graph, dilute the sample test solution in the mobile phase and repeat the measurement step. Identify the nitrate or
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