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 [1].
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von anorganischem Arsen in Lebensmitteln marinen Ursprungs und pflanzlichen Lebensmitteln mit Anionenaustausch-HPLC-ICP-MS
Diese Europäische Norm beschreibt ein Verfahren zur Bestimmung von anorganischem Arsen in marinen und pflanzlichen Lebensmitteln mit Anionenaustausch-HPLC-ICP-MS nach Wasserbadextraktion.
Dieses Verfahren wurde in einem Ringversuch an Reis (poliert), Vollkornreis, Porree (Lauch), Miesmuscheln, Fischfleisch und Meeresalgen mit einem Massenanteil an anorganischem Arsen von 0,073 mg/kg bis 10,3 mg/kg [1] 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
Overview
EN 16802:2016 is a CEN European Standard that specifies a validated laboratory method for the determination of inorganic arsenic in foodstuffs of marine and plant origin. The method combines waterbath extraction (dilute HNO3 / H2O2) with anion‑exchange HPLC coupled to ICP‑MS (HPLC‑ICP‑MS) for selective separation and quantification of arsenate (As(V)) after oxidation of arsenite (As(III)). The procedure was validated in an interlaboratory study on matrices such as white and wholemeal rice, leek, blue mussels, fish muscle and seaweed across an inorganic arsenic range of 0.073 mg/kg to 10.3 mg/kg.
Key Topics and Requirements
- Scope and principle
- Extraction of arsenic species using 0.1–0.2 mol/L HNO3 with 3–6% H2O2 and heated waterbath (90 °C ± 2 °C) for 60 min ± 5 min.
- Oxidation of As(III) to As(V) to allow selective measurement of total inorganic arsenic as arsenate.
- Separation by strong anion exchange (SAX) HPLC and detection by ICP‑MS.
- Reagents and mobile phase
- Ultra‑pure water (ISO 3696 grade 1), high‑purity nitric acid and hydrogen peroxide.
- Example mobile phase: 50 mmol/L ammonium carbonate in 3% methanol, pH 10.3 (matrix and column dependent).
- Instrumentation and consumables
- HPLC system with SAX column (guard column recommended), ICP‑MS (argon ≥ 99.99%), centrifuge (≥ 2 010 g), waterbath, filtration (0.45 µm), analytical balance (±1 mg).
- Quality control and calibration
- External, matrix‑matched calibration using extraction solution for standards to prevent species interconversion.
- Blank control and chromatographic checks (organic arsenic separation, chloride elution to avoid 40Ar35Cl+ interference).
- Contamination control & safety
- Use of sub‑boiled acids, clean lab practices, avoidance of glass where possible; safety warning for hazardous reagents and equipment.
Applications - Who should use EN 16802:2016
- Food testing laboratories performing regulatory monitoring of inorganic arsenic in rice, seaweed, seafood and plant‑derived foods.
- Regulatory agencies and public health laboratories validating compliance with contaminant limits and food safety standards.
- Research institutions studying arsenic speciation, human exposure, and food chain transfer.
- Quality assurance teams in food industry labs implementing validated speciation techniques.
Practical uses include routine surveillance, method validation, risk assessment inputs, and producing defensible data for regulatory enforcement or product safety declarations.
Related Standards
- EN 13804 - General considerations and specific requirements for element/species determinations in foodstuffs.
- EN ISO 3696 - Water for analytical laboratory use (quality of water required for reagents and dilutions).
Keywords: EN 16802:2016, inorganic arsenic, HPLC‑ICP‑MS, anion‑exchange HPLC, waterbath extraction, arsenic speciation, food analysis, rice, seaweed, mussels.
Frequently Asked Questions
EN 16802:2016 is a standard published by the European Committee for Standardization (CEN). Its full title is "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 standard covers: 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 [1].
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 [1].
EN 16802:2016 is classified under the following ICS (International Classification for Standards) categories: 67.050 - General methods of tests and analysis for food products; 67.060 - Cereals, pulses and derived products; 67.120.30 - Fish and fishery products. The ICS classification helps identify the subject area and facilitates finding related standards.
EN 16802:2016 is associated with the following European legislation: EU Directives/Regulations: 882/2004; Standardization Mandates: M/422. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.
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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
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
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
Precision data . 11 Annex B (informative)
Supplementary information about chromatographic conditions . 12 Bibliography . 13
°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
· 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
...
Die Norm EN 16802:2016 bietet eine präzise und methodisch fundierte Vorgehensweise zur Bestimmung von anorganischem Arsen in Lebensmitteln pflanzlicher und maritimer Herkunft. Der Umfang dieser europäischen Norm umfasst die Durchführung von Anionenaustausch-HPLC-ICP-MS-Analysen, die nach einer Wasserbad-Extraktion erfolgen. Diese Methodik ist insbesondere für die Untersuchung einer Vielzahl von Lebensmitteln geeignet, darunter Vollkornreis, Lauch, Miesmuscheln, Fischmuskel und Algen. Ein herausragendes Merkmal der Norm ist die Validierung der Methode durch interlaboratorische Tests, die eine hohe Zuverlässigkeit und Reproduzierbarkeit der Ergebnisse gewährleisten. Der nachgewiesene Gehalt an anorganischem Arsen reicht dabei von 0,073 mg/kg bis zu 10,3 mg/kg, was die Norm besonders relevant für die Lebensmittelsicherheit und die Überwachung von Schadstoffbelastungen in Lebensmitteln macht. Die Standardisierung in EN 16802:2016 ist entscheidend für die Gewährleistung von Schutzmaßnahmen in der Lebensmittelindustrie, da anorganisches Arsen als ein potenzielles Gesundheitsrisiko angesehen wird. Diese Norm ermöglicht es Laboratories, die gesetzlichen Vorschriften zur Lebensmittelüberwachung präzise einzuhalten und trägt somit zur Verbesserung der Lebensmittelsicherheit bei. Insgesamt bietet die EN 16802:2016 eine robuste und verlässliche Methode, um anorganisches Arsen in verschiedenen Lebensmitteln zu bestimmen, und ist daher von großer Bedeutung für die Lebensmittelanalytik und den Verbraucherschutz.
표준 문서 EN 16802:2016은 해양 및 식물 기원 식품에서 무기 비소를 결정하는 방법을 제시하고 있습니다. 이 표준의 범위는 수욕 추출 후 이온 교환 HPLC-ICP-MS를 이용하여 무기 비소를 정량하는 절차를 포함합니다. 이 방법은 백미, 통밀 쌀, 리크, 블루 홍합, 생선 근육 및 해조류에 대해 0.073 mg/kg에서 10.3 mg/kg까지의 무기 비소 질량 비율을 갖는 샘플에 대해 상호 실험실 테스트에서 검증되었습니다. 이 표준의 강점은 해양 및 식물 기원 식품에서의 무기 비소를 정확히 측정할 수 있다는 점입니다. 특히, HPLC-ICP-MS 기술을 활용한 이 방법은 매우 민감하고 정밀하며, 다양한 식품 매트릭스에서 적용 가능하다는 장점이 있습니다. 또한, 이 표준은 실험실 간 비교 가능성을 보장하여 식품 안전 및 품질 관리를 향상시킵니다. EN 16802:2016 표준은 식품 분석 및 안전성 검증에 있어 매우 중요한 역할을 하며, 이를 통해 소비자에게 안전한 식품을 제공하는 데 기여하고 있습니다. 따라서 이 표준은 규제 기관 및 식품 산업에 있어 필수적인 기준이 됩니다. 무기 비소의 정확한 측정은 인체 건강과 관련된 여러 문제를 예방하는 데 중요한 요소로 작용하며, 이 표준이 제시하는 방법론은 이러한 필요에 부응하고 있습니다.
EN 16802:2016の標準文書は、食品における無機ヒ素の定量に関する重要なガイドラインを提供しています。このドキュメントの範囲は、海洋および植物由来の食品における無機ヒ素の測定方法を、陰イオン交換HPLC-ICP-MSという高度な分析技術を用いて詳述しています。水浴抽出に続くこの手法は、無機ヒ素の正確な定量を可能にし、食品安全の確保に寄与します。 この標準の強みは、異なる食品サンプルにおける無機ヒ素の評価に対する厳密なバリデーションです。具体的には、白米、全粒米、ネギ、青ムール貝、魚筋肉、海藻の計測において、0.073 mg/kgから10.3 mg/kgの範囲で無機ヒ素の質量分率が確認されています。この幅広い食品に対する適用可能性は、さまざまな消費者の食事におけるリスク評価を行う上で非常に重要です。 また、EN 16802:2016の関連性は、EUの食品安全基準の遵守を求める法的要求に合わせており、持続可能な食の取り組みを支える役割も果たしています。この標準は、食品産業における無機ヒ素管理の必要性を認識した上で、業界全体の信頼性向上につながるため、特に重要です。食品製造業者、検査機関、規制当局にとって、必須の参考資料となるでしょう。
La norme SIST EN 16802:2016 offre une approche rigoureuse pour la détermination de l'arsenic inorganique dans les denrées alimentaires d'origine marine et végétale par la méthode HPLC-ICP-MS avec échange d'anions. Son étendue couvre des matrices variées, incluant le riz blanc, le riz complet, le poireau, les moules bleues, la chair de poisson et les algues, attestant de la polyvalence de la méthode pour différents types d'aliments. L'un des points forts de cette norme réside dans son processus de validation interlaboratoire, qui assure une fiabilité et une reproductibilité des résultats. Les tests effectués sur des échantillons avec une fraction massique d'arsenic inorganique variant de 0,073 mg/kg à 10,3 mg/kg confirment l'efficacité de la méthode dans une plage de concentration pertinente pour le contrôle de la sécurité alimentaire. Cela est particulièrement pertinent dans le contexte actuel où la sécurité alimentaire et la santé publique sont des priorités. De plus, la méthode d'extraction par bain-marie suivie de l'analyse par HPLC-ICP-MS offre un équilibre optimal entre complexité technique et efficacité analytique, ce qui démontre sa pertinence pour les laboratoires d'analyses. La norme se positionne comme un outil essentiel pour les professionnels du secteur alimentaire, leur permettant de garantir que les produits respectent les limites réglementaires concernant l'arsenic inorganique. En conclusion, la norme SIST EN 16802:2016 est non seulement pertinente pour l'analyse de la contamination par l'arsenic inorganique dans des aliments variés, mais elle contribue également à l'harmonisation des méthodes analytiques au sein de l'Union européenne, renforçant ainsi la confiance des consommateurs et promouvant la sécurité alimentaire.
The standard EN 16802:2016 offers a comprehensive framework for the determination of inorganic arsenic in foodstuffs of marine and plant origin through anion-exchange HPLC-ICP-MS. Its well-defined scope addresses the critical need for accurate measurement of inorganic arsenic levels in various food matrices such as white rice, wholemeal rice, leek, blue mussels, fish muscle, and seaweed. The specified mass fraction range of 0.073 mg/kg to 10.3 mg/kg underscores the standard's rigor in ensuring the reliability of results across typical concentrations found in these food products. One of the key strengths of this standard is its validation through an interlaboratory test, which adds credibility and ensures that the procedure can be consistently reproduced across different testing environments. This aspect is vital given the growing concerns about food safety and the potential health impacts of inorganic arsenic consumption. Moreover, the utilization of anion-exchange HPLC coupled with ICP-MS for detection demonstrates the standard's alignment with cutting-edge analytical techniques, enhancing the sensitivity and specificity of the measurements. The relevance of EN 16802:2016 extends beyond regulatory compliance; it serves as an essential tool for food safety authorities, laboratories, and researchers aiming to monitor and control arsenic levels in food products. By providing a standardized methodology, the document plays a pivotal role in supporting public health initiatives and ensuring consumer safety regarding food quality. Overall, EN 16802:2016 is a vital standard that leverages scientific advancements to address contemporary food safety challenges effectively.
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