SIST EN 16802:2016
(Main)Foodstuffs - Determination of elements and their chemical species - Determination of inorganic arsenic in foodstuffs of marine and plant origin by anion-exchange HPLC-ICP-MS
Foodstuffs - Determination of elements and their chemical species - Determination of inorganic arsenic in foodstuffs of marine and plant origin by anion-exchange HPLC-ICP-MS
This draft European Standard describes a procedure for the determination of inorganic arsenic in foodstuffs of marine and plant origin by anion-exchange HPLC-ICP-MS following waterbath extraction.
This method has been validated in an interlaboratory test on white rice, wholemeal rice, leek, blue mussels, fish muscle and seaweed with an inorganic arsenic mass fraction in the range 0,073 mg/kg to 10,3 mg/kg.
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von anorganischem Arsen in Lebensmitteln marinen Ursprungs und pflanzlichen Lebensmitteln mit Anionenaustausch-HPLC-ICP-MS
Der Entwurf dieser Europäischen Norm beschreibt ein Verfahren zur Bestimmung von anorganischem Arsen in Lebensmitteln marinen Ursprungs und pflanzlichen Lebensmitteln mit Anionenaustausch-HPLC-ICP-MS nach Wasserbadextraktion.
Dieses Verfahren wurde in einem Ringversuch an Weißreis, Vollkornreis, Porree (Lauch), Miesmuscheln, Fischmuskel und Meeresalgen mit einem Massenanteil des anorganischen Arsens im Bereich von 0,073 mg/kg bis 10,3 mg/kg validiert.
Produits alimentaires - Détermination des éléments et de leurs espèces chimiques - Détermination de la teneur en arsenic inorganique dans les produits alimentaires d'origines marine et végétale, par CLHP avec échange d'anions et spectrométrie de masse à plasma induit par haute fréquence (ICP-SM)
Le présent projet de Norme européenne spécifie un mode opératoire de détermination de la teneur en arsenic inorganique dans les produits alimentaires d’origines marine et végétale par HPLC à échange d'anions ICP MS après extraction par bain d'eau.
Cette méthode a été validée dans le cadre d’un essai interlaboratoires réalisé sur du riz blanc, du riz complet, du poireau, des moules bleues, du muscle de poisson et du varech dont la teneur massique en arsenic inorganique est comprise entre 0,073 mg/kg et 10,3 mg/kg.
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje anorganskega arzena v živilih morskega in rastlinskega izvora z anionsko izmenjavo HPLC-ICP-MS
Ta osnutek evropskega standarda opisuje postopek za določevanje anorganskega arzena v živilih morskega in rastlinskega izvora z anionsko izmenjavo HPLC-ICP-MS po ekstrakciji v vodni kopeli.
Ta metoda je bila potrjena z medlaboratorijskim preskusom belega riža, polnozrnatega riža, pora, užitnih klapavic, mišičnine rib in morskih alg z masnim deležem anorganskega arzena v območju od 0,073 mg/kg do 10,3 mg/kg.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.þHYDQMHQLRQVNRLebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von anorganischem Arsen in Lebensmitteln marinen Ursprungs und pflanzlichen Lebensmitteln mit Anionenaustausch-HPLC-ICP-MSProduits alimentaires - Détermination des éléments et de leurs espèces chimiques - Détermination de la teneur en arsenic inorganique dans les produits alimentaires d'origines marine et végétale, par CLHP avec échange d'anions et spectrométrie de masse à plasma induit par haute fréquence (ICP-SM)Foodstuffs - Determination of elements and their chemical species - Determination of inorganic arsenic in foodstuffs of marine and plant origin by anion-exchange HPLC-ICP-MS67.120.30Ribe in ribji proizvodiFish and fishery products67.060QMLKCereals, pulses and derived products67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 16802:2016SIST EN 16802:2016en,fr,de01-junij-2016SIST EN 16802:2016SLOVENSKI
STANDARD
SIST EN 16802:2016
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16802
March
t r s x ICS
x yä r w râ
x yä r x râ
x yä s t rä u r English Version
Foodstuffs æ Determination of elements and their chemical species æ Determination of inorganic arsenic in foodstuffs of marine and plant origin by anionæexchange HPLCæICPæMS Produits alimentaires æ Détermination des éléments et de leurs espèces chimiques æ Détermination de la teneur en arsenic inorganique dans les produits alimentaires d 5origines marine et végétaleá par CLHP avec échange d 5anions et spectrométrie de masse à
Lebensmittel æ Bestimmung von Elementen und ihren Verbindungen æ Bestimmung von anorganischem Arsen in Lebensmitteln marinen Ursprungs und pflanzlichen Lebensmitteln mit AnionenaustauschæHPLCæICPæMS This European Standard was approved by CEN on
z February
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x z r tã t r s x ESIST EN 16802:2016
EN 16802:2016 (E) 2 Contents Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Principle . 4 4 Reagents . 4 5 Apparatus and equipment . 6 6 Procedure. 7 6.1 General . 7 6.2 Waterbath extraction . 7 6.3 Determination of inorganic arsenic by HPLC-ICP-MS . 7 6.3.1 Preparation of HPLC-ICP-MS for analysis . 7 6.3.2 Calibration . 8 6.3.3 Determination of samples and blank solution . 8 6.3.4 HPLC sequence . 8 6.3.5 Typical HPLC-ICP-MS settings . 8 6.4 Quality control . 9 7 Calculation . 9 7.1 Integration of peaks . 9 7.2 Inorganic arsenic in test solutions . 9 7.3 Calculation of inorganic arsenic in the samples . 9 8 Precision . 10 8.1 General . 10 8.2 Repeatability . 10 8.3 Reproducibility . 10 9 Test report . 10 Annex A (informative)
Precision data . 11 Annex B (informative)
Supplementary information about chromatographic conditions . 12 Bibliography . 13
SIST EN 16802:2016
EN 16802:2016 (E) 3 European foreword This document (EN 16802:2016) 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 September 2016, and conflicting national standards shall be withdrawn at the latest by September 2016. 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. This document has been prepared under mandate M 422 given to CEN by the European Commission and the European Free Trade Association. 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, Former Yugoslav Republic of Macedonia, 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 16802:2016
EN 16802:2016 (E) 4 1 Scope This European Standard describes a procedure for the determination of inorganic arsenic in foodstuffs of marine and plant origin by anion-exchange HPLC-ICP-MS following waterbath extraction. This method has been validated in an interlaboratory test on white rice, wholemeal rice, leek, blue mussels, fish muscle and seaweed with an inorganic arsenic mass fraction in the range 0,073 mg/kg to 10,3 mg/kg [1]. 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 13804, Foodstuffs — Determination of elements and their chemical species — General considerations and specific requirements EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) 3 Principle This standard describes a method for the determination of inorganic arsenic. Inorganic arsenic consists of arsenite, As(III) and arsenate, As(V). A representative test portion of the sample is treated with a diluted nitric acid and hydrogen peroxide solution in a heated waterbath. Hereby the arsenic species are extracted into solution and As(III) is oxidized to As(V). The inorganic arsenic is selectively separated from other arsenic compounds using anion exchange HPLC (High Performance Liquid Chromatography) coupled online to the element-specific detector ICP-MS (Inductively Coupled Plasma Mass Spectrometry) for the determination of the mass fraction of inorganic arsenic. External calibration with solvent matrix-matched standards is used for quantification of the amount of inorganic arsenic. WARNING — The use of this standard can 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 its use. 4 Reagents 4.1 General The concentration of the arsenic species in the reagents and water used shall be low enough to not affect the results of the determination. When using a method of high sensitivity like ICP-MS, the control of the blank levels of water, acid and other reagents is very important. Generally ultra-pure water complying with ISO 3696 grade 1 (i.e. electrical conductivity below 0,1
°C) and acid of high purity, e.g. cleaned by sub-boiling distillation, are recommended. Reagents should be of minimum p.a. quality where possible. Special facilities can be used in order to avoid contamination during the steps of preparation and measurement (e.g. uses of laminar flow benches or comparable clean room facilities). 4.2 Nitric acid concentrated, mass fraction w(HNO3),
· 65 %, mass concentration of approximately (HNO3) = 1,4 g/ml. Use only nitric acid available with high purity or perform a clean-up by a sub-boiling distillation in order to avoid potential contamination. SIST EN 16802:2016
EN 16802:2016 (E) 5 4.3 Hydrogen peroxide, w(H2O2 %. High purity is essential to avoid potential contamination. Commercially available hydrogen peroxide for analysis should be tested for contamination of arsenic. 4.4 Extraction solution 1, c(HNO3) = 0,1 mol/l in 3 %(V/V) H2O2. Pour 800 ml of H2O and then 6,5 ml of HNO3 (4.2) and thereafter 100 ml of H2O2 (4.3) into a 1 000 ml volumetric flask. Fill it up to the mark with H2O. This solution should be prepared on the same day of use. It is recommended that the total volume needed for the analysis is estimated and only this amount is produced. 4.5 Extraction solution 2, c(HNO3) = 0,2 mol/l in 6 % (V/V) H2O2. Pour 70 ml of H2O, 1,3 ml of nitric acid (4.2) and 20 ml of hydrogen peroxoide (4.3) into a 100 ml volumetric flask. Fill up to the mark at 100 ml with H2O. This solution should be prepared on the same day of use. It is recommended that the total volume needed for the analysis is estimated and only this amount is produced. 4.6 Ammonium carbonate, w[(NH4)2CO3]
· 99,999 %, for production of mobile phase solution. 4.7 Aqueous ammonia, w[NH3(aq.)]
· 25 %, for adjustment of pH in the mobile phase. 4.8 Methanol, (CH3OH), HPLC grade, for production of mobile phase. 4.9 Mobile phase, e.g. 50 mmol/l ammonium carbonate in 3 % methanol at pH 10,3. Dissolve e.g. 4,80 g of ammonium carbonate (4.6) in approximately 800 ml of water. Adjust the pH to 10,3 with aqueous ammonia (4.7), add 30 ml of methanol (4.8) and fill up to 1 000 ml with water. Filter the mobile phase solution through a 0,45 µm filter prior to use. The optimal concentration of ammonium carbonate in the mobile phase depends on the analytical column used (e.g. brand, particle size and dimensions). The appropriate concentration of ammonia carbonate is at the discretion of the analyst and should fulfil the criteria for sufficient resolution of the arsenate peak as stated in 5.10. Methanol is added to the mobile phase in order to enhance the signal intensity for arsenic (carbon enhancement effect [2]). The concentration of methanol for maximum signal depends on the instrument used and should be identified by the analyst. 4.10 Diarsenic trioxide, w(As2O3)
· 99,5 %, optional. 4.11 Potassium hydroxide solution, (KOH) = 20 g/100 ml, optional. 4.12 Sulfuric acid solutions, w(H2SO4) = 20 % and w(H2SO4) = 1 %, optional. 4.13 Phenolphthalein, optional. 4.14 Standard solutions, with an arsenic mass concentration of 1 000 mg/l. The use of commercial standards of arsenic, arsenic III and/or V, with a mass concentration of 1 000 mg/l is recommended. SIST EN 16802:2016
EN 16802:2016 (E) 6 Otherwise proceed as follows: Dissolve e.g. 1,320 g of diarsenic trioxide (4.10) in 25 ml of potassium hydroxide solution (4.11), neutralize with 20 % sulfuric acid solution (4.12) with phenolphthalein (4.13) as indicator and dilute to 1 000 ml in a volumetric flask with 1 % sulfuric acid solution (4.12). NOTE By preparing the standard in the extraction solution 1 (4.4) all arsenite will be completely oxidized to arsenate. 4.15 Calibration solutions. Prepare a range of standards including a blank calibration solution that covers the linear range of the analyte to be determined by diluting the analyte stock solution with extraction solution 1 (4.4). Appropriate matrix matching of the calibration solutions shall be performed by using the extraction solution 1 (4.4) for the final dilution step, which furthermore will prevent reduct
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