EN 17266:2019
(Main)Foodstuffs - Determination elements and their chemical species - Determination of organomercury in seafood by elemental mercury analysis
Foodstuffs - Determination elements and their chemical species - Determination of organomercury in seafood by elemental mercury analysis
This document describes a method for the determination of organomercury in seafood/fishery products by elemental mercury analysis. The method has been successfully valideted in an interlaboratory study with a working range from 0,013 mg/kg to 5,12 mg/kg (HORRAT values <2) in seafood/fishery products [1], [2]. The limit of quantification is approximately 0,010 mg/kg organomercury (referring to dry weight, expressed as mercury) [3], [4].
Organic species of mercury, other than monomethylmercury, are also extracted and thus determined with this method. However, in seafood/fishery products the contribution from organic species of mercury other than monomethylmercury is negligible.
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von Organoquecksilber in Fisch und Meeresfrüchten mittels Feststoffquecksilberbestimmung
Dieses Dokument legt ein Verfahren zur Bestimmung von Organoquecksilber in Fisch und Meeresfrüchten durch Nutzung eines Quecksilber Feststoff Analysators fest. Das Verfahren wurde in einem Ringversuch an Austerngewebe, Muschelgewebe, Hummer Hepatopankreas, Hundshaileber und Thunfisch mit Mengen von 0,01 mg/kg bis 5 mg/kg (bezogen auf das Trockengewicht und als Quecksilber ausgedrückt) erfolgreich validiert [1], [2].
Die Bestimmungsgrenze liegt bei etwa 0,01 mg/kg Organoquecksilber[3], [4].
Andere organische Quecksilberspezies als Monomethylquecksilber werden ebenfalls extrahiert und somit mit diesem Verfahren bestimmt. Bei Fisch und Meeresfrüchten ist der Beitrag anderer organischer Quecksilberspezies neben Monomethylquecksilber jedoch vernachlässigbar.
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage du mercure organique dans les produits de la mer par analyse du mercure élémentaire
La présente Norme européenne spécifie une méthode de dosage du mercure organique dans les produits
de la mer par analyse du mercure élémentaire. La méthode a été validée au cours d’un essai
interlaboratoires sur du tissu d’huître, du tissu de moule, de l’hépatopancréas de homard, du foie de
roussette et du thon à des niveaux allant de 0,01 mg/kg à 5 mg/kg faisant référence au poids sec et
exprimés en tant que mercure [1], [2].
La limite de quantification est d’environ 0,01 mg/kg de mercure organique [3], [4].
Les espèces organiques du mercure, autres que le monométhylmercure, sont également extraites et ainsi
dosées avec cette méthode. Cependant, dans les produits de la mer, la contribution des espèces
organiques du mercure autres que le monométhylmercure est négligeable.
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje organskih živosrebrovih spojin v morski hrani z analizo elementarnega živega srebra
Ta dokument opisuje metodo za določanje organskega živega srebra v morskih /ribiških proizvodih z elementarno analizo živega srebra. Metoda je bila uspešno potrjena v medlaboratorijski študiji z delovnim obsegom od 0,013 mg/kg do 5,12 mg/kg (vrednosti HORRAT < 2) v morskih sadežih/ribiških proizvodih [1], [2]. Meja količinskega določanja je približno 0,010 mg/kg organskega živega srebra (ki se navezuje na suho maso, izraženo kot živo srebro) [3], [4]. Organske vrste živega srebra, razen monometilnega živega srebra, se tudi ekstrahirajo in tako določijo s to metodo. Vendar pa je v morskih/ribiških proizvodih prispevek organskih vrst živega srebra, razen monometilnega živega srebra, zanemarljiv.
General Information
Overview - EN 17266:2019 (CEN)
EN 17266:2019 specifies a validated method for the determination of organomercury in seafood and fishery products using elemental mercury analysis (direct/automated mercury analyser). The method was validated in interlaboratory studies on matrices such as oyster, mussel, lobster hepatopancreas, dogfish liver and tuna. Reported performance includes a working range of approximately 0.013 mg/kg to 5.12 mg/kg (HORRAT values < 2) and a limit of quantification (LOQ) ≈ 0.010 mg/kg (dry weight, expressed as Hg). Alternative detection techniques may be used if equivalence of performance is demonstrated.
Key topics and technical requirements
- Principle: double liquid–liquid extraction (toluene then L‑cysteine) to isolate organomercury, followed by thermal decomposition and detection with an elemental mercury analyser. Mercury is trapped on a gold amalgamator and detected by atomic absorption at 253.7 nm.
- Scope of species: method extracts organic mercury species generally; in seafood the contribution of organic Hg species other than monomethylmercury (MMHg) is negligible.
- Validated matrices and range: validated across molluscs, crustaceans, fish tissues and livers with the above working range and LOQ.
- Reagents and cleanliness: requires low‑mercury reagents (HNO3, HCl, HBr, toluene, L‑cysteine), and careful labware cleaning per EN 13804 to minimize blanks.
- Instrumentation and consumables: elemental mercury analyser (cells for small volumes), centrifuge, analytical balance, PP/vials; calibration is notably stable (often up to one year) but must be checked after component changes.
- Quality control: internal QC solutions (QC1/QC2), calibration curve acceptance, instrument verification, recovery checks and contamination control are specified.
- Precision: interlaboratory validation data and repeatability/reproducibility performance are provided (informative annex).
Practical applications and users
- Who uses it: food control and public health laboratories, seafood processors, aquaculture labs, environmental and research laboratories, and regulatory agencies monitoring seafood safety.
- Applications:
- Regulatory compliance testing for organomercury / monomethylmercury in seafood.
- Routine surveillance and monitoring programs for mercury in fish and shellfish.
- Research on mercury bioaccumulation and exposure assessment.
- Verification of processing or sourcing strategies to reduce mercury exposure.
Related standards
- 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.
Keywords: EN 17266:2019, organomercury, seafood testing, elemental mercury analysis, monomethylmercury, LOQ 0.010 mg/kg, direct mercury analyser, CEN, food safety.
Frequently Asked Questions
EN 17266:2019 is a standard published by the European Committee for Standardization (CEN). Its full title is "Foodstuffs - Determination elements and their chemical species - Determination of organomercury in seafood by elemental mercury analysis". This standard covers: This document describes a method for the determination of organomercury in seafood/fishery products by elemental mercury analysis. The method has been successfully valideted in an interlaboratory study with a working range from 0,013 mg/kg to 5,12 mg/kg (HORRAT values <2) in seafood/fishery products [1], [2]. The limit of quantification is approximately 0,010 mg/kg organomercury (referring to dry weight, expressed as mercury) [3], [4]. Organic species of mercury, other than monomethylmercury, are also extracted and thus determined with this method. However, in seafood/fishery products the contribution from organic species of mercury other than monomethylmercury is negligible.
This document describes a method for the determination of organomercury in seafood/fishery products by elemental mercury analysis. The method has been successfully valideted in an interlaboratory study with a working range from 0,013 mg/kg to 5,12 mg/kg (HORRAT values <2) in seafood/fishery products [1], [2]. The limit of quantification is approximately 0,010 mg/kg organomercury (referring to dry weight, expressed as mercury) [3], [4]. Organic species of mercury, other than monomethylmercury, are also extracted and thus determined with this method. However, in seafood/fishery products the contribution from organic species of mercury other than monomethylmercury is negligible.
EN 17266:2019 is classified under the following ICS (International Classification for Standards) categories: 67.120.30 - Fish and fishery products. The ICS classification helps identify the subject area and facilitates finding related standards.
EN 17266:2019 is associated with the following European legislation: EU Directives/Regulations: 882/2004. 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)
SLOVENSKI STANDARD
01-januar-2020
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje organskih
živosrebrovih spojin v morski hrani z analizo elementarnega živega srebra
Foodstuffs - Determination elements and their chemical species - Determination of
organomercury in seafood by elemental mercury analysis
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Organoquecksilber in Fisch- und Meeresfrüchten mit Feststoffquecksilberbestimmung
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage du
mercure organique dans les fruits de mer par analyse du mercure élémentaire
Ta slovenski standard je istoveten z: EN 17266:2019
ICS:
67.120.30 Ribe in ribji proizvodi Fish and fishery products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 17266
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2019
EUROPÄISCHE NORM
ICS 67.120.30
English Version
Foodstuffs - Determination elements and their chemical
species - Determination of organomercury in seafood by
elemental mercury analysis
Produits alimentaires - Dosage des éléments et de leurs Lebensmittel - Bestimmung von Elementen und ihren
espèces chimiques - Dosage du mercure organique Verbindungen - Bestimmung von Organoquecksilber in
dans les produits de la mer par analyse du mercure Fisch und Meeresfrüchten mittels Elementaranalyse
élémentaire von Quecksilber
This European Standard was approved by CEN on 9 September 2019.
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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17266:2019 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 5
6 Apparatus and equipment . 7
7 Procedure. 8
7.1 Sample preparation . 8
7.2 Reagent blank solution . 8
7.3 Determination by elemental mercury analyser . 8
7.4 Instrumental parameters . 9
7.5 Analytical sequence . 9
8 Quality control . 9
8.1 Recovery . 9
8.2 Instrument verification . 10
8.3 Calibration curve . 10
8.4 Absence of contamination . 11
9 Evaluation . 11
9.1 Calculation . 11
9.2 Expression of results . 11
10 Precision . 11
10.1 General . 11
10.2 Repeatability . 11
10.3 Reproducibility . 11
11 Test report . 12
Annex A (informative) Precision data . 13
Bibliography . 15
European foreword
This document (EN 17266:2019) 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 May 2020, and conflicting national standards shall be
withdrawn at the latest by May 2020.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: 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, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
1 Scope
This document specifies a method for the determination of organomercury in seafood by elemental
mercury analysis. The method has been successfully validated in an interlaboratory study on oyster
tissue, mussel tissue, lobster hepatopancreas, dogfish liver and tuna at levels from 0,01 mg/kg to
5 mg/kg referring to dry weight and expressed as mercury [1], [2].
The limit of quantification is approximately 0,01 mg/kg of organomercury [3], [4].
Organic species of mercury, other than monomethylmercury, are also extracted and thus determined
with this method. However, in seafood the contribution from organic species of mercury other than
monomethylmercury is negligible.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. 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 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at http://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
4 Principle
Organomercury in seafood/fishery products is separated from the matrix by double liquid-liquid
extraction, first with an organic solvent (toluene) and subsequently with L-cysteine solution and is
determined by elemental mercury analyser [3], [4].
Elemental mercury analyser, also known as automated or direct mercury analyser, is a single purpose
atomic absorption spectrophotometer for mercury determination. The determination of mercury with
an elemental mercury analyser is based on sample drying and subsequent thermal decomposition,
including electro thermal atomisation of mercury. A gold amalgamator selectively traps and pre-
concentrates the mercury from the flow of decomposition products. Finally, the trapped mercury is
thermally released and detected by atomic absorption at 253,7 nm. Organomercury results are
expressed in mg/kg as mercury.
Alternative detection techniques can be used, provided that equivalence of method performance is
proven.
5 Reagents
The mass concentration of mercury in the reagents and water used shall be low enough not to affect the
results. All reagents shall be of analytical grade, i.e. pro analysis, p.a. or similar unless otherwise
specified.
Use water conforming to grade 2 of EN ISO 3696.
5.1 Nitric acid, mass fraction, w (HNO ) = 65 % (m/m), density approximately 1,4 g/ml
5.2 Hydrochloric acid, w (HCl) = 32 % (m/m), density approximately 1,18 g/ml
5.3 Diluted hydrochloric acid solution
Mix equal volumes of hydrochloric acid (5.2) and water.
5.4 Hydrobromic acid, w (HBr) approximately 47 %, density approximately 1,47 g/ml
5.5 Toluene
1)
5.6 L-cysteine monohydrate hydrochloride, e.g. Ph. Eur. or USP grade
5.7 Sodium sulfate anhydrous
5.8 Sodium acetate anhydrous
5.9 L-cysteine solution, mass concentration ρ = 1 g/100 ml
Weigh 1,0 g of L-cysteine monohydrate hydrochloride (5.6), 12,5 g of sodium sulfate (5.7) and 0,8 g of
sodium acetate (5.8) into a 100 ml beaker. Add about 75 ml of water and stir until complete dissolution.
Transfer this solution completely to a 100 ml volumetric flask and make up to volume with water. This
solution can be stored for 1 day at ambient temperature. Other preparation volumes may be used as
long as proportions are kept.
The mass concentration of mercury in the L-cysteine solution should be as low as possible. The purity of
this solution should be such that the response for mercury shall be less than half the response of the
1 µg/l mercury standard solution (calibration solution 1, see 5.13).
L-cysteine precipitates on the catalytic tube which should thus be changed or cleaned as appropriate.
5.10 Mercury stock solution, ρ(Hg) = 1 000 mg/l Hg
5.11 Monomethylmercury (MMHg) chloride, minimum purity of 95 %
5.12 Mercury standard solutions
5.12.1 Mercury standard solution 1 (ρ = 10 mg/l Hg)
Pipette 1,0 ml of the commercial mercury stock solution 1 000 mg/l Hg (5.10) in a 100 ml volumetric
flask, add 2,0 ml of diluted hydrochloric acid solution (5.3) and make up to volume with water. This
solution is stable in a glass container in the refrigerator at approximately 2 °C to 10 °C for 6 months.
5.12.2 Mercury standard solution 2 (ρ = 0,50 mg/l Hg)
1)
Ph. Eur. = European Pharmacopoeia; USP = United States Pharmacopoeia.
Pipette 2,5 ml of mercury standard solution 1 (5.12.1) in a 50 ml volumetric flask, add 1,0 ml of diluted
hydrochloric acid solution (5.3) and make up to volume with water. This solution is stable in a glass
container in the refrigerator at approximately 2 °C to 10 °C for 2 months.
5.13 Calibration solutions
Due to the highly stable response of elemental mercury analysers, there is no need to recalibrate for
each analytical sequence. Calibration is usually stable for at least 1 year. For that reason every
instrumental calibration will be maintained for that period, provided that quality controls for each
sequence are satisfactory. Nevertheless, if the gold amalgamator or catalyst tube is changed, response
could change and a new calibration is necessary. In such a case, analyse 500 µl of each calibration
solution (from blank to 100 µg/l Hg). For selection of corresponding calibration solutions for each
calibration curve, see 7.4. For acceptance criteria regarding the calibration curve, see 8.3.
Select calibration solutions depending on the cell used, thus on the expected concentration level of the
sample. This is comprehensively described in 7.4.
Prepare all calibration solutions freshly for each calibration.
Other volumes of preparation are suitable provided that they maintain the proportions described
below. Pipette either mercury standard solution 2 (5.12.2) or calibration solution 7 (see Table 1) in a
50 ml volumetric flask and fill up to the mark with L-cysteine solution (5.9) according to the scheme
presented in Table 1.
Use L-cysteine solution (5.9) as blank (level 0) for calibration.
Table 1 — Example of calibration solutions
Volume of initial Final Hg
Calibration solution
solution concentration (ρ)
Initial solution
no
ml µg/l
0 L-cysteine solution (5.9) 50 0
1 calibration solution no 7 1,0 1,0
2 calibration solution no 7 2,5 2,5
3 standard solution 2 (5.12.2) 0,5 5,0
4 standard solution 2 (5.12.2) 1,0 10
5 standard solution 2 (5.12.2) 1,5 15
6 standard solution 2 (5.12.2) 2,5 25
7 standard solution 2 (5.12.2) 5,0 50
8 standard solution 2 (5.12.2) 7,5 75
9 standard solution 2 (5.12.2) 10,0 100
5.14 Internal quality control solutions
5.14.1 General
As the response of elemental mercury analysers is highly stable, there is no need to recalibrate the
instrument for each analytical sequence. However, some control solutions are used to ensure the
validity of the latest calibration. Each calibration curve needs to be compared against an external
solution to demonstrate absence of error in intermediate calibration solutions preparation.
...
SLOVENSKI STANDARD
01-januar-2020
Živila - Določevanje elementov in njihovih kemijskih oblik - Določevanje organskih
živosrebrovih spojin v morski hrani z analizo elementarnega živega srebra
Foodstuffs - Determination elements and their chemical species - Determination of
organomercury in seafood by elemental mercury analysis
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Organoquecksilber in Fisch- und Meeresfrüchten mit Feststoffquecksilberbestimmung
Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage du
mercure organique dans les fruits de mer par analyse du mercure élémentaire
Ta slovenski standard je istoveten z: EN 17266:2019
ICS:
67.120.30 Ribe in ribji proizvodi Fish and fishery products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 17266
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2019
EUROPÄISCHE NORM
ICS 67.120.30
English Version
Foodstuffs - Determination elements and their chemical
species - Determination of organomercury in seafood by
elemental mercury analysis
Produits alimentaires - Dosage des éléments et de leurs Lebensmittel - Bestimmung von Elementen und ihren
espèces chimiques - Dosage du mercure organique Verbindungen - Bestimmung von Organoquecksilber in
dans les produits de la mer par analyse du mercure Fisch und Meeresfrüchten mittels Elementaranalyse
élémentaire von Quecksilber
This European Standard was approved by CEN on 9 September 2019.
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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17266:2019 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 5
6 Apparatus and equipment . 8
7 Procedure. 8
7.1 Sample preparation . 8
7.2 Reagent blank solution . 8
7.3 Determination by elemental mercury analyser . 8
7.4 Instrumental parameters . 9
7.5 Analytical sequence . 9
8 Quality control . 9
8.1 Recovery . 9
8.2 Instrument verification . 10
8.3 Calibration curve . 10
8.4 Absence of contamination . 11
9 Evaluation . 11
9.1 Calculation . 11
9.2 Expression of results . 11
10 Precision . 11
10.1 General . 11
10.2 Repeatability . 11
10.3 Reproducibility . 11
11 Test report . 12
Annex A (informative) Precision data . 13
Bibliography . 15
European foreword
This document (EN 17266:2019) 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 May 2020, and conflicting national standards shall be
withdrawn at the latest by May 2020.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: 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, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
1 Scope
This document specifies a method for the determination of organomercury in seafood by elemental
mercury analysis. The method has been successfully validated in an interlaboratory study on oyster
tissue, mussel tissue, lobster hepatopancreas, dogfish liver and tuna at levels from 0,01 mg/kg to
5 mg/kg referring to dry weight and expressed as mercury [1], [2].
The limit of quantification is approximately 0,01 mg/kg of organomercury [3], [4].
Organic species of mercury, other than monomethylmercury, are also extracted and thus determined
with this method. However, in seafood the contribution from organic species of mercury other than
monomethylmercury is negligible.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. 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 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at http://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
4 Principle
Organomercury in seafood/fishery products is separated from the matrix by double liquid-liquid
extraction, first with an organic solvent (toluene) and subsequently with L-cysteine solution and is
determined by elemental mercury analyser [3], [4].
Elemental mercury analyser, also known as automated or direct mercury analyser, is a single purpose
atomic absorption spectrophotometer for mercury determination. The determination of mercury with
an elemental mercury analyser is based on sample drying and subsequent thermal decomposition,
including electro thermal atomisation of mercury. A gold amalgamator selectively traps and pre-
concentrates the mercury from the flow of decomposition products. Finally, the trapped mercury is
thermally released and detected by atomic absorption at 253,7 nm. Organomercury results are
expressed in mg/kg as mercury.
Alternative detection techniques can be used, provided that equivalence of method performance is
proven.
5 Reagents
The mass concentration of mercury in the reagents and water used shall be low enough not to affect the
results. All reagents shall be of analytical grade, i.e. pro analysis, p.a. or similar unless otherwise
specified.
Use water conforming to grade 2 of EN ISO 3696.
5.1 Nitric acid, mass fraction, w (HNO ) = 65 % (m/m), density approximately 1,4 g/ml
5.2 Hydrochloric acid, w (HCl) = 32 % (m/m), density approximately 1,18 g/ml
5.3 Diluted hydrochloric acid solution
Mix equal volumes of hydrochloric acid (5.2) and water.
5.4 Hydrobromic acid, w (HBr) approximately 47 %, density approximately 1,47 g/ml
5.5 Toluene
1)
5.6 L-cysteine monohydrate hydrochloride, e.g. Ph. Eur. or USP grade
5.7 Sodium sulfate anhydrous
5.8 Sodium acetate anhydrous
5.9 L-cysteine solution, mass concentration ρ = 1 g/100 ml
Weigh 1,0 g of L-cysteine monohydrate hydrochloride (5.6), 12,5 g of sodium sulfate (5.7) and 0,8 g of
sodium acetate (5.8) into a 100 ml beaker. Add about 75 ml of water and stir until complete dissolution.
Transfer this solution completely to a 100 ml volumetric flask and make up to volume with water. This
solution can be stored for 1 day at ambient temperature. Other preparation volumes may be used as
long as proportions are kept.
The mass concentration of mercury in the L-cysteine solution should be as low as possible. The purity of
this solution should be such that the response for mercury shall be less than half the response of the
1 µg/l mercury standard solution (calibration solution 1, see 5.13).
L-cysteine precipitates on the catalytic tube which should thus be changed or cleaned as appropriate.
5.10 Mercury stock solution, ρ(Hg) = 1 000 mg/l Hg
5.11 Monomethylmercury (MMHg) chloride, minimum purity of 95 %
5.12 Mercury standard solutions
5.12.1 Mercury standard solution 1 (ρ = 10 mg/l Hg)
Pipette 1,0 ml of the commercial mercury stock solution 1 000 mg/l Hg (5.10) in a 100 ml volumetric
flask, add 2,0 ml of diluted hydrochloric acid solution (5.3) and make up to volume with water. This
solution is stable in a glass container in the refrigerator at approximately 2 °C to 10 °C for 6 months.
5.12.2 Mercury standard solution 2 (ρ = 0,50 mg/l Hg)
1)
Ph. Eur. = European Pharmacopoeia; USP = United States Pharmacopoeia.
Pipette 2,5 ml of mercury standard solution 1 (5.12.1) in a 50 ml volumetric flask, add 1,0 ml of diluted
hydrochloric acid solution (5.3) and make up to volume with water. This solution is stable in a glass
container in the refrigerator at approximately 2 °C to 10 °C for 2 months.
5.13 Calibration solutions
Due to the highly stable response of elemental mercury analysers, there is no need to recalibrate for
each analytical sequence. Calibration is usually stable for at least 1 year. For that reason every
instrumental calibration will be maintained for that period, provided that quality controls for each
sequence are satisfactory. Nevertheless, if the gold amalgamator or catalyst tube is changed, response
could change and a new calibration is necessary. In such a case, analyse 500 µl of each calibration
solution (from blank to 100 µg/l Hg). For selection of corresponding calibration solutions for each
calibration curve, see 7.4. For acceptance criteria regarding the calibration curve, see 8.3.
Select calibration solutions depending on the cell used, thus on the expected concentration level of the
sample. This is comprehensively described in 7.4.
Prepare all calibration solutions freshly for each calibration.
Other volumes of preparation are suitable provided that they maintain the proportions described
below. Pipette either mercury standard solution 2 (5.12.2) or calibration solution 7 (see Table 1) in a
50 ml volumetric flask and fill up to the mark with L-cysteine solution (5.9) according to the scheme
presented in Table 1.
Use L-cysteine solution (5.9) as blank (level 0) for calibration.
Table 1 — Example of calibration solutions
Volume of initial Final Hg
Calibration solution
solution concentration (ρ)
Initial solution
no
ml µg/l
0 L-cysteine solution (5.9) 50 0
1 calibration solution no 7 1,0 1,0
2 calibration solution no 7 2,5 2,5
3 standard solution 2 (5.12.2) 0,5 5,0
4 standard solution 2 (5.12.2) 1,0 10
5 standard solution 2 (5.12.2) 1,5 15
6 standard solution 2 (5.12.2) 2,5 25
7 standard solution 2 (5.12.2) 5,0 50
8 standard solution 2 (5.12.2) 7,5 75
9 standard solution 2 (5.12.2) 10,0 100
5.14 Internal quality control solutions
5.14.1 General
As the response of elemental mercury analysers is highly stable, there is no need to recalibrate the
instrument for each analytical sequence. However, some control solutions are used to ensure the
validity of the latest calibration. Each calibration curve needs to be compared against an external
solution to demonstrate absence of error in intermediate calibration s
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The standard EN 17266:2019 provides a comprehensive framework for the determination of organomercury in seafood and fishery products through elemental mercury analysis. Its scope clearly defines a method that is both robust and precise, having been validated through an interlaboratory study, demonstrating a working range from 0.013 mg/kg to 5.12 mg/kg, with HORRAT values less than 2, which indicates a high level of reliability in results across different laboratories. One of the primary strengths of this standard lies in its ability to quantify organomercury levels with a limit of quantification of approximately 0.010 mg/kg in dry weight, making it particularly useful for regulators and seafood industry stakeholders concerned with food safety and compliance. The inclusion of the capability to extract and determine organic species of mercury beyond monomethylmercury enhances the richness of data that can be obtained from seafood samples, despite the negligible contribution from these other organic forms in practical applications. The relevance of EN 17266:2019 is underscored by the increasing global scrutiny on seafood safety and mercury content, ensuring that consumers receive safe and uncontaminated food sources. By standardizing the method for detecting organomercury, this document plays a critical role in promoting public health, supporting environmental regulations, and enabling monitoring of seafood quality. Overall, the EN 17266:2019 standard not only provides a validated and reliable methodology for the determination of organomercury but also supports broader initiatives aimed at improving food safety in the seafood sector.
La norme EN 17266:2019, intitulée "Aliments - Détermination des éléments et de leurs espèces chimiques - Détermination de l'organomercure dans les produits de la mer par analyse de mercure élémentaire", présente une méthode innovante et pertinente pour l'analyse de l'organomercure dans les produits de la mer. L'étendue de cette norme est clairement définie, spécifiant qu'elle s'applique à la détermination de l'organomercure dans les produits de pêche et de mer. La méthode a été validée avec succès lors d'une étude interlaboratoire, mettant en évidence une plage de travail fiable allant de 0,013 mg/kg à 5,12 mg/kg, avec des valeurs HORRAT inférieures à 2, ce qui indique une robustesse considérable dans la répétabilité des résultats. La limite de quantification de l'organomercure est d'environ 0,010 mg/kg, ce qui est crucial pour assurer la sécurité alimentaire et la protection des consommateurs. Une force importante de cette norme réside dans sa capacité à extraire et déterminer également d'autres espèces organiques de mercure, bien que dans le contexte des produits de la mer, le contribution de ces espèces autres que le monométhylmercure soit négligeable. Cela souligne l'exhaustivité de la méthode, garantissant que l'analyse est précise et complète pour les produits marins. En somme, la norme EN 17266:2019 joue un rôle fondamental dans le cadre de l'évaluation de la sécurité des aliments, particulièrement pour les produits de la mer, en établissant un protocole fiable pour la détermination de l'organomercure. Sa pertinence est indiscutable dans le contexte actuel de préoccupation croissante autour des contaminations métalliques dans les aliments, renforçant ainsi sa contribution significative à la santé publique et à la régulation des comportements alimentaires.
La norme EN 17266:2019 constitue un document essentiel pour la détermination des éléments et de leurs espèces chimiques dans les produits de la mer, spécifiquement pour l'organo-mercury. Cette norme fournit une méthode validée pour l'analyse du mercure élémentaire dans les produits de la pêche, permettant ainsi de garantir la sécurité alimentaire. L'étendue de la méthode est bien définie, avec une plage de travail allant de 0,013 mg/kg à 5,12 mg/kg, ce qui démontre son efficacité et sa précision dans le cadre d'études interlaboratoires, où les valeurs HORRAT sont inférieures à 2. Un point fort de cette norme est son seuil de quantification, établi à environ 0,010 mg/kg pour l'organo-mercury, ce qui est crucial pour le contrôle de la qualité des produits de la mer. Ce seuil est basé sur le poids sec et s'exprime en mercure, offrant ainsi une référence claire pour les professionnels de l'industrie alimentaire. De plus, la norme prend en compte les espèces organiques de mercure, même si, dans le contexte des produits de la mer, leur contribution est jugée négligeable par rapport au monométhylmercure. La pertinence de la norme EN 17266:2019 réside dans son application directe pour garantir que les produits de la mer soient conformes aux réglementations de sécurité alimentaire. En assurant une méthode rigoureuse et standardisée pour évaluer la présence de l'organo-mercury, cette norme représente un atout majeur pour les laboratoires analytiques et les acteurs de l'industrie de la pêche, contribuant à protéger la santé publique tout en soutenant la confiance des consommateurs.
標準化文書SIST EN 17266:2020は、魚介類における有機水銀の定量を行うための的方法論を示しています。この標準は、元素水銀分析を用いており、0.013 mg/kgから5.12 mg/kgの範囲で有効性が確認されたことから、信頼性の高い分析手法として位置づけられています（HORRAT値<2）。このことは、食品安全の観点から非常に重要です。 本標準の強みは、十分に検証された分析手法が提供されている点にあります。具体的には、定量の限界が約0.010 mg/kgであり、これは乾燥重量で表される水銀に関連しています。これにより、非常に低い濃度でも正確な測定が可能であり、消費者保護に貢献します。 さらに、有機水銀の他の種も抽出可能であるため、包括的な成分分析が行える点も評価できます。ただし、実際の魚介類においては、モノメチル水銀以外の有機水銀種の寄与は無視できるほど小さいことも記されています。このように、標準は特にモノメチル水銀の安全性評価において重要な役割を果たします。 この文書は、魚介類製品の安全性を確保し、消費者に安心を提供するための基準として、高い関連性を持つといえます。全体として、SIST EN 17266:2020は、食品物質における有機水銀の定量において、確固たる基盤を提供する有意義な規範です。
EN 17266:2019は、海産物に含まれる有機水銀の分析方法を定義した重要な標準規格です。この文書では、元素水銀分析を用いた海産物および水産物における有機水銀の定量方法が詳細に説明されています。特に、この方法は、0.013 mg/kgから5.12 mg/kgの範囲で、他の研究機関との間で行われたインターロンタイアリー研究によって成功裏にバリデーションが行われており、再現性が非常に良好であることが示されています（HORRAT値が2未満である点が強調されています）。 この標準の強みは、比較的低い有機水銀の定量限界を特徴としており、約0.010 mg/kg（乾燥重量換算）という感度での分析が可能です。これは、海産物の安全性を確保するために非常に重要です。また、モノメチル水銀以外の有機水銀種もこの方法で抽出されており、全体的な水銀負荷の理解を深めることに寄与しています。ただし、海産物や水産物中のモノメチル水銀以外の有機水銀種の寄与は極めて微小であるため、実際の分析では主にモノメチル水銀に着目しています。 このEN 17266:2019の文書は、海産物における水銀汚染の監視と評価において非常に実用的かつ重要なリソースであり、食品業界や環境監視機関における信頼性の高い情報提供に寄与することが期待されます。そのため、海産物の安全性規制を遵守するためには、この標準の導入と活用が不可欠です。
SIST EN 17266:2020 표준은 해양 식품 및 수산물에서 유기 수은의 측정을 위한 방법을 체계적으로 제시하고 있습니다. 이 문서는 원자 수은 분석을 통한 유기 수은의 검출 방법을 상세히 설명하며, 해양식품/수산물에 대한 인터래버러토리 연구를 통해 성공적으로 검증되었습니다. 검증된 작업 범위는 0.013 mg/kg에서 5.12 mg/kg까지이며, HORRAT 값이 2 미만으로 안정성을 보장합니다. 이 표준의 강점 중 하나는 유기 수은의 양적 한계를 명확하게 제시한 점입니다. 측정의 양적 한계는 약 0.010 mg/kg으로 정의되며 이는 건조 중량 기준으로 수은으로 표현됩니다. 또한, 이 방법은 모노메틸 수은 외의 유기 수은 종도 추출하여 측정할 수 있으나, 수산물에서는 모노메틸 수은 외의 유기 수은 기여도가 미미하다는 점에서 이 표준의 실용성이 강조됩니다. 따라서 SIST EN 17266:2020 표준은 해양 식품 및 수산물에서 유기 수은을 안전하고 정확하게 측정할 수 있는 신뢰할 수 있는 도구로서, 관련 분야에서는 반드시 참고해야 할 중요한 문서입니다.
Die Norm EN 17266:2019 bietet einen umfassenden Rahmen für die Bestimmung von Organomerkur in Meeresfrüchten und fischereilichen Produkten durch die Analyse von elementarem Merkur. Die Definition eines soliden Verfahrens zur Analyse von gefährlichen Stoffen in Lebensmitteln ist von großer Bedeutung, insbesondere im Hinblick auf die Lebensmittelsicherheit und den Schutz der Verbraucher. Die methodischen Ansätze in der Norm wurden erfolgreich in einer Interlaboratorienstudie validiert, was die Zuverlässigkeit und Reproduzierbarkeit der Ergebnisse unterstreicht. Mit einem Arbeitsbereich von 0,013 mg/kg bis 5,12 mg/kg (HORRAT-Werte <2) belegt die Norm ihre Stärke und Anwendbarkeit in der praktischen Durchführung von Analysen in der Lebensmittelbranche. Der Quantifizierungsgrenzwert von etwa 0,010 mg/kg für Organomerkur (bezogen auf das Trockengewicht, ausgedrückt als Quecksilber) stellt sicher, dass auch minimale Mengen erfasst werden können und somit der Gesundheitsrisikomanagement-Prozess unterstützt wird. Ein weiterer Vorteil der Norm ist, dass neben Monomethylquecksilber auch andere organische Spezies von Quecksilber extrahiert und bestimmt werden können. Obwohl der Beitrag dieser anderen organischen Quecksilberspezies in Meeresfrüchten vernachlässigbar ist, zeigt dies doch die Breite der Methodenanwendung und die Möglichkeit der umfassenden Analyse von Schadstoffen in Lebensmitteln. Die Relevanz von EN 17266:2019 in der heutigen Lebensmittelindustrie kann nicht hoch genug eingeschätzt werden. Angesichts der anhaltenden Bedenken hinsichtlich Quecksilberkontaminationen in Fischereiprodukten unterstützt die Norm die Einhaltung internationaler Sicherheitsstandards und fördert das Vertrauen der Verbraucher. Die Sicherstellung einer genauen und präzisen Bestimmung von Organomerkur schafft eine klare Grundlage für weitere Forschungs- und Entwicklungsmöglichkeiten in der Lebensmittelanalytik.
Die Norm EN 17266:2019 befasst sich mit der Bestimmung von Organomercury in Meeresfrüchten und Fischereiprodukten durch die Analyse von elementarem Quecksilber. Die Relevanz dieser Norm ist besonders hoch, da sie eine präzise Methode zur Identifizierung und Quantifizierung von Organomercury bietet, die für die Lebensmittelsicherheit von entscheidender Bedeutung ist. Der Umfang der Norm ist klar definiert: Sie beschreibt das Verfahren zur Bestimmung von Organomercury in einer Vielzahl von Meeresfrüchte- und Fischereiprodukten, was die Anwendbarkeit der Methode in der Praxis unterstreicht. Die erfolgreiche Validierung der Methode in einer interlaborativen Studie, mit einem Arbeitsbereich von 0,013 mg/kg bis 5,12 mg/kg und HORRAT-Werten von unter 2, zeigt die hohe Zuverlässigkeit und Präzision der Norm. Zudem liegt die Nachweisgrenze bei etwa 0,010 mg/kg Organomercury, was für die Überwachung und Kontrolle von Quecksilber in Lebensmitteln von großer Bedeutung ist. Ein weiterer positiver Aspekt dieser Norm ist, dass auch organische Quecksilberspezies, abgesehen von Monomethylquecksilber, extrahiert und bestimmt werden. Es wird jedoch darauf hingewiesen, dass der Beitrag anderer organischer Quecksilberspezies in Meeresfrüchten vernachlässigbar ist, was die Fokussierung auf Monomethylquecksilber weiter legitimiert. Insgesamt stellt die EN 17266:2019 eine wesentliche Grundlage für die Kenntnis und Kontrolle von Organomercury in Meeresfrüchten dar, die sowohl für die Industrie als auch für Vereinbarungen zur Lebensmittelsicherheit von großer Bedeutung ist. Es wird empfohlen, diese Norm als Maßstab für künftige Analysen zu verwenden, um sicherzustellen, dass die Anforderungen an die Sicherheit der Lebensmittel eingehalten werden.
EN 17266:2019 표준은 해산물 및 수산물에서 유기수은을 분석하기 위한 중요한 방법론을 제시합니다. 이 문서는 원소 수은 분석법을 통해 해산물에서 유기수은을 결정하는 방법에 대해 상세히 설명하고 있습니다. 이 표준의 범위는 0.013 mg/kg에서 5.12 mg/kg까지의 작업 범위를 가지며, HORRAT 값이 2 이하인 대규모 interlaboratory 연구에서 성공적으로 검증되었습니다. 이는 해산물 및 수산물의 품질 보증을 위한 신뢰성 있는 분석 방법임을 나타냅니다. EN 17266:2019의 강점 중 하나는 정량 한계가 약 0.010 mg/kg으로 설정되어 있어 매우 낮은 농도의 유기수은도 감지할 수 있는 능력을 가진다는 점입니다. 이는 해산물의 안전성을 보장하고 소비자 보호에 기여하는 중요한 요소입니다. 또한 이 방법은 단일 메틸수은 이외에도 다른 유기 수은 종을 추출하고 분석할 수 있지만, 해산물에서 단일 메틸수은 이외의 유기 수은 종의 기여는 미미하다는 점을 명시하고 있습니다. 해양 식품의 안전성을 높이기 위한 이 표준은 해산물 소비자들에게 재료의 품질 및 안전성을 보장하는 데 매우 중요하며, 식품 산업 종사자들에게도 필수적인 지침으로 작용합니다. 전체적으로 EN 17266:2019는 해산물 품질 관리를 위한 실용적이고 효과적인 표준으로서의 역할을 다하고 있으며, 해양 식품에서 유기수은의 신뢰성 있는 분석을 위해 계속해서 활용될 것입니다.
The standard EN 17266:2019, focused on the determination of organomercury in seafood via elemental mercury analysis, serves a crucial role in ensuring food safety and public health. This standard outlines a well-structured methodology for assessing organomercury content in seafood and fishery products, reflecting its significant scope in the field of aquatic food analysis. The strengths of this standard lie in its rigorous validation process, demonstrated through an interlaboratory study that confirmed the method's reliability. With a working range from 0.013 mg/kg to 5.12 mg/kg and HORRAT values below 2, this indicates high precision and reproducibility in measuring organomercury levels. Moreover, the limit of quantification at approximately 0.010 mg/kg for organomercury (calculated on a dry weight basis) underscores the sensitivity of this analytical approach, making it highly suitable for routine monitoring in food safety. Furthermore, it is noteworthy that the method is capable of extracting and determining various organic mercury species, despite the negligible contribution of species other than monomethylmercury in seafood. This comprehensive analysis ensures that even minimal contaminant levels are accurately accounted for, thereby reinforcing the standard's relevance in regulatory compliance and consumer protection. Overall, EN 17266:2019 stands out as a vital standard in food safety analysis, providing essential guidelines for the determination of organomercury in seafood, thereby supporting both industry practices and consumer health.
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