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Abstract

Fifty-nine samples of wild caught fishery products and crustaceans were collected between March 2023 – February 2024 from Kilkeel Fish Market in Northern Ireland. Forty-four of the samples were analysed for the contaminants: mercury, lead and cadmium (heavy metals). The other fifteen samples were tested for dioxins and PCBs:

  • 1,2,3,4,6,7,8-HeptaCDD
  • 1,2,3,4,6,7,8-HeptaCDF
  • 1,2,3,4,7,8,9-HeptaCDF
  • 1,2,3,4,7,8-HexaCDD
  • 1,2,3,4,7,8-HexaCDF
  • 1,2,3,6,7,8-HexaCDD
  • 1,2,3,6,7,8-HexaCDF
  • 1,2,3,7,8,9-HexaCDD
  • 1,2,3,7,8,9-HexaCDF
  • 1,2,3,7,8-PentaCDD
  • 1,2,3,7,8-PentaCDF
  • 2,3,4,6,7,8-HexaCDF
  • 2,3,4,7,8-PentaCDF
  • 2,3,7,8-TetraCDD
  • 2,3,7,8-TetraCDF
  • OctaCDD
  • OctaCDF

and PCBs (dioxin-like and non-dioxin-like PCBs included for analysis)

  • PCB 28 (2,4,4′-Trichlorobiphenyl) *
  • PCB 52 (2,2′,5,5′-Tetrachlorobiphenyl) *
  • PCB 77 (3,3′,4,4′-Tetrachlorobiphenyl, 3,3′,4,4′-PCB)
  • PCB 81 (3,4,4’,5-Tetrachlorobiphenyl)
  • PCB 101 (2,2′,4,5,5′-Pentachlorobiphenyl) *
  • PCB 105 (2,3,3′,4,4′-Pentachlorobiphenyl)
  • PCB 114 (2,3,4,4’,5-Pentachlorobiphenyl)
  • PCB 118
  • PCB 123
  • PCB 126
  • PCB 138 (2,2′,3,4,4′,5′-Hexachlorobiphenyl) *
  • PCB 153 (2,2′,4,4′,5,5′-Hexachlorobiphenyl) *
  • PCB 156 (2,3,3′,4,4′,5-Hexachlorobiphenyl)
  • PCB 157
  • PCB 167
  • PCB 169
  • PCB 180 (2,2′,3,4,4′,5,5′-Heptachlorobiphenyl) *
  • PCB 189

*non-dioxin-like PCBs.

Concentrations of mercury, lead and cadmium were less than the maximum EU regulatory limits for all samples tested.

Concentrations of dioxins and PCBs were below the EU regulatory limits for these compounds.

1. Introduction

1.1 Background to the study

Eurofins Food Testing Ireland Ltd (Public Analysts) was contracted by the Food Standards Agency (FSA) in Northern Ireland to assess the levels of various chemical contaminants (heavy metals, dioxins and polychlorinated biphenyls (PCBs)) in a number of species of wild caught fishery products and crustaceans landed in Northern Ireland between March 2023 and February 2024.

1.2. Aims and objectives of the study

The official control surveillance programme is undertaken to comply with Article 70 of Commission Implementing Regulation (EU) 2019/627 (EU, 2019) which requires a monitoring programme to be established for wild caught fishery products to control compliance with EU legislation on contaminants. Commission Regulation (EU) 2023/915 on maximum levels for certain contaminants in food and repealing Regulation (EC) No 1881/2006 (EU, 2023), sets down the maximum levels for certain contaminants in food, including fishery products.

The data has the potential to provide support to certifying officers in their attestation of the compliance of wild caught fishery products landed in Northern Ireland with contaminants legislation when signing Export Health Certificates.

The aim of the work was to determine concentrations of defined chemical contaminants in wild caught fishery products to assess whether the levels were within the limits prescribed (EU, 2023) and were safe for placing on the market.

2. Material and methods

2.1. Samples

Fifty-nine samples of wild caught fishery products and crustaceans were collected from 22nd March 2023 to 21st February 2024 from Kilkeel Fish Market in Northern Ireland (Annex A). Forty-four of the samples were analysed for the contaminants: mercury, lead and cadmium (heavy metals). The other fifteen samples were tested for dioxins and PCBs. To plan the purchase and collection of samples, FSA in Northern Ireland shared a list of required products with authorised officers from Newry Mourne and Down District Council, for random sampling.

The type and number of samples of each species collected for analyses were determined based on the quantity of that species landed in Northern Ireland, and any previous exceedances. The species sampled included:

  • Dublin Bay Prawn

  • Mackerel

  • Haddock

  • Brown crab

  • Herring

  • King scallop

On receipt at the laboratory (Eurofins Food Testing Ireland Ltd, Dublin, Ireland) each sample was assigned a unique laboratory reference number, and the sample details were logged into a database.

2.2. Sample preparation

For fin fish, samples were filleted to collect edible muscle tissue and exclude skin, bones and organs. For crustacea, only the white meat was taken to represent the sample. The selected tissue was homogenised in a blender. The aliquots for either metals or dioxins/PCBs analyses were immediately weighed out and the remaining material was stored in a freezer.

2.3. Metal Analysis

Samples were analysed for cadmium, mercury and lead using an in-house (Eurofins WEJ Contaminants GmbH) method based on EN ISO 15763: Determination of trace elements - determination of cadmium, mercury and lead in foodstuffs by Inductively coupled plasma mass spectrometry (ICP-MS) after pressure digestion.

Aliquots of homogenised test sample material were digested in an acid solution using a high-pressure microwave system. The solution was diluted as required before analysis. Quantification of the four elements was by ICP-MS.

The analysis is accredited to ISO 17025, with the inclusion of certified and in-house reference materials and method blanks which were evaluated prior to the reporting of sample data and were used to determine the limits of quantification.

2.4. Dioxin and PCB analysis

Samples were prepared for analysis using a cold extraction method and analysed for dioxins and PCBs using methods by Eurofins Lab Zeeuws-Vlaanderen outlined in Commission Regulation (EU) 2017/644 (EU, 2017). The following analytes were determined:

Dioxins:

  • 1,2,3,4,6,7,8-HeptaCDD

  • 1,2,3,4,6,7,8-HeptaCDF

  • 1,2,3,4,7,8,9-HeptaCDF

  • 1,2,3,4,7,8-HexaCDD

  • 1,2,3,4,7,8-HexaCDF

  • 1,2,3,6,7,8-HexaCDD

  • 1,2,3,6,7,8-HexaCDF

  • 1,2,3,7,8,9-HexaCDD

  • 1,2,3,7,8,9-HexaCDF

  • 1,2,3,7,8-PentaCDD

  • 1,2,3,7,8-PentaCDF

  • 2,3,4,6,7,8-HexaCDF

  • 2,3,4,7,8-PentaCDF

  • 2,3,7,8-TetraCDD

  • 2,3,7,8-TetraCDF

  • OctaCDD

  • OctaCDF

Dioxin-like PCBs:

  • PCB 77 (3,3′,4,4′-Tetrachlorobiphenyl, 3,3′,4,4′-PCB)
  • PCB 81 (3,4,4’,5-Tetrachlorobiphenyl)

  • PCB 105 (2,3,3′,4,4′-Pentachlorobiphenyl)

  • PCB 114 (2,3,4,4’,5-Pentachlorobiphenyl)

  • PCB 118

  • PCB 123

  • PCB 126

  • PCB 156 (2,3,3′,4,4′,5-Hexachlorobiphenyl)

  • PCB 157

  • PCB 167

  • PCB 169

  • PCB 189

Non-dioxin-like PCBs:

  • PCB 28 (2,4,4′-Trichlorobiphenyl)

  • PCB 52 (2,2′,5,5′-Tetrachlorobiphenyl)

  • PCB 101 (2,2′,4,5,5′-Pentachlorobiphenyl)

  • PCB 138 (2,2′,3,4,4′,5′-Hexachlorobiphenyl)

  • PCB 153 (2,2′,4,4′,5,5′-Hexachlorobiphenyl)

  • PCB 180 (2,2′,3,4,4′,5,5′-Heptachlorobiphenyl)

The value of each congener was multiplied by its World Health Organisation-Toxicity Equivalent Factor (WHO-TEFs). The product was presented as the Toxic Equivalency (TEQ).

  • Lower-bound: the concept which requires using zero for the contribution of each congener <Limit of Quantification (LOQ).

  • Medium-bound: the concept which requires using half of the limit of quantification calculating the contribution of each congener < LOQ.

  • Upper-bound: the concept which requires using the limit of quantification for the contribution of each congener < LOQ.

The analysis is accredited to ISO 17025. Each sample is analysed with the addition of certified standards. The recovery of the standards is checked in each sample against the EU regulation (EU) 2017/644 (EU, 2017). The LOQ is dependent on the LOD, sample weight and sample matrix.

3. Results and discussion

The concentrations of the contaminants measured in the fifty-nine samples were determined by Eurofins and were compared to limits prescribed in Commission Regulation (EU) 2023/915 (EU, 2023).

3.1. Metals analysis

Concentrations of mercury, cadmium and lead were below the regulatory limits for these compounds and are provided in Table 1 in Annex B.

3.2. Dioxin and PCB analysis

Concentrations of dioxins and PCBs were below the regulatory limits for these compounds and are provided in Table 2 in Annex B.

Acknowledgements

Fera Science Ltd.

  • Title: Chemical contaminants in wild caught fishery products and crustaceans 2023-2024 – Northern Ireland

  • Customer: Food Standards Agency – Northern Ireland

  • FSA NI Project Officer: Annmarie O’Toole

  • Report Number: Report FR/002638-88

  • Fera Project: Number FR/002638-8

  • Compiled by: Emma Bradley

  • Authorised by: Susan MacDonald

Note: Fera shall not be responsible for confirming or ascertaining the accuracy or completeness of any information or data provided by customer or by any third party on its behalf. Accordingly, any advice given by Fera, or its representatives based on such information or data, including any results contained in any reports and/or any recommendations, interpretation, analysis, guidance, suggestions, proposals, endorsements given by Fera in connection with the services, are given without liability on the part of Fera.

This report has been prepared by Fera after exercise of all reasonable care and skill but is provided without liability in its application and use. This report may not be reproduced except in full, without the written approval of Fera. Whilst care has been taken to ensure that the web links contained in this report are correct at the time of issue, changes may occur.

Copyright © Fera Science Ltd. (Fera) 2024

References

EU. (2017). Commission Regulation (EU) 2017/644 of 5 April 2017 laying down methods of sampling and analysis for the control of levels of dioxins, dioxin-like PCBs and non-dioxin-like PCBs in certain foodstuffs and repealing Regulation (EU) No 589/2014. https:/​/​eur-lex.europa.eu/​legal-content/​EN/​TXT/​PDF/​?uri=CELEX:32017R0644
EU. (2019). Commission Implementing Regulation (EU) 2019/627 of 15 March 2019 laying down uniform practical arrangements for the performance of official controls on products of animal origin intended for human consumption in accordance with Regulation (EU) 2017/625 of the European Parliament and of the Council and amending Commission Regulation (EC) No 2074/2005 as regards official controls. https:/​/​eur-lex.europa.eu/​eli/​reg_impl/​2019/​627/​oj
EU. (2023). Commission Regulation (EU) 2023/915 of 25 April 2023 on maximum levels for certain contaminants in food and repealing Regulation (EC) No 1881/2006. https:/​/​eur-lex.europa.eu/​legal-content/​en/​TXT/​?uri=CELEX%3A32023R0915

Annexes

Annex A: Sample details

Sample number Full Product Text Description Landing date Fish Market
FSAWF61 King Scallop 18.04.2023 Kilkeel Fish Market
FSAWF62 King Scallop 24.04.2023 Kilkeel Fish Market
FSAWF63 King Scallop 29.04.2023 Kilkeel Fish Market
FSAWF64 Nephrops 22.08.2023 Kilkeel Fish Market
FSAWF65 Nephrops 22.06.2023 Kilkeel Fish Market
FSAWF66 Nephrops 23.06.2023 Kilkeel Fish Market
FSAWF67 Nephrops 22.06.2023 Kilkeel Fish Market
FSAWF68 Nephrops 25.04.2023 Kilkeel Fish Market
FSAWF69 Nephrops 23.06.2023 Kilkeel Fish Market
FSAWF70 Nephrops 28.04.2023 Kilkeel Fish Market
FSAWF71 Brown Crab 26.08.2023 Kilkeel Fish Market
FSAWF72 Nephrops 28.08.2023 Kilkeel Fish Market
FSAWF73 Nephrops 29.08.2023 Kilkeel Fish Market
FSAWF74 Mackerel 30.08.2023 Kilkeel Fish Market
FSAWF75 Brown Crab 21.08.2023 Kilkeel Fish Market
FSAWF76 Herring 15.08.2023 Kilkeel Fish Market
FSAWF77 Brown Crab 17.08.2023 Kilkeel Fish Market
FSAWF78 Brown Crab 06.08.2023 Kilkeel Fish Market
FSAWF79 Brown Crab 23.03.2023 Kilkeel Fish Market
FSAWF80 Brown Crab 16.08.2023 Kilkeel Fish Market
FSAWF81 Nephrops 16.07.2023 Kilkeel Fish Market
FSAWF82 Nephrops 29.05.2023 Kilkeel Fish Market
FSAWF83 Brown Crab 16.05.2023 Kilkeel Fish Market
FSAWF84 Brown Crab 22.03.2023 Kilkeel Fish Market
FSAWF85 Brown Crab 24.04.2023 Kilkeel Fish Market
FSAWF86 King Scallop 17.04.2023 Kilkeel Fish Market
Sample number Full Product Text Description Landing date Fish Market
FSAWF87 Herring 16.08.2023 Kilkeel Fish Market
FSAWF88 Herring 16.08.2023 Kilkeel Fish Market
FSAWF89 Herring 29.08.2023 Kilkeel Fish Market
FSAWF90 Mackerel 31.08.2023 Kilkeel Fish Market
FSAWF91 Mackerel 13.09.2023 Kilkeel Fish Market
FSAWF92 King Scallop 16.06.2023 Kilkeel Fish Market
FSAWF93 Herring 07.09.2023 Kilkeel Fish Market
FSAWF94 Herring 05.09.2023 Kilkeel Fish Market
FSAWF95 Mackerel 15.09.2023 Kilkeel Fish Market
FSAWF96 Haddock 11.09.2023 Kilkeel Fish Market
FSAWF97 Herring 14.09.2023 Kilkeel Fish Market
FSAWF98 Mackerel 11.09.2023 Kilkeel Fish Market
FSAWF99 Herring 15.09.2023 Kilkeel Fish Market
FSAWF100 Herring 15.11.2023 Kilkeel Fish Market
FSAWF101 Herring 13.11.2023 Kilkeel Fish Market
FSAWF102 Herring 26.11.2023 Kilkeel Fish Market
FSAWF103 Herring 17.01.2024 Kilkeel Fish Market
FSAWF104 Herring 17.01.2024 Kilkeel Fish Market
FSAWF105 Herring 23.01.2024 Kilkeel Fish Market
FSAWF106 Herring 23.01.2024 Kilkeel Fish Market
FSAWF107 Herring 30.01.2024 Kilkeel Fish Market
FSAWF108 Herring 30.01.2024 Kilkeel Fish Market
FSAWF109 Herring 14.12.2023 Kilkeel Fish Market
FSAWF110 Herring 15.12.2023 Kilkeel Fish Market
FSAWF111 Herring 15.12.2023 Kilkeel Fish Market
FSAWF112 Haddock 09.11.2023 Kilkeel Fish Market
FSAWF113 Mackerel 16.02.2024 Kilkeel Fish Market
FSAWF114 Mackerel 21.02.2024 Kilkeel Fish Market
Sample number Full Product Text Description Landing date Fish Market
FSAWF115 Mackerel 24.01.2024 Kilkeel Fish Market
FSAWF116 Mackerel 24.01.2024 Kilkeel Fish Market
FSAWF117 Mackerel 01.02.2024 Kilkeel Fish Market
FSAWF118 Mackerel 13.02.2024 Kilkeel Fish Market
FSAWF119 Mackerel 21.2.2024 Kilkeel Fish Market

Annex B: Tables

Table 1. Mercury, cadmium and lead concentrations in wild caught fishery products and crustaceans

Concentrations are not corrected for recovery.

Brown Crab
Sample number Species Mercury (mg/kg) Cadmium (mg/kg) Lead
(mg/kg)
FSAWF75 Brown Crab 0.049 0.17 < 0.02
FSAWF77 Brown Crab 0.16 0.092 < 0.02
FSAWF78 Brown Crab 0.14 0.28 < 0.02
FSAWF79 Brown Crab 0.16 0.15 < 0.02
FSAWF80 Brown Crab 0.046 0.030 < 0.02
FSAWF83 Brown Crab 0.052 < 0.005 < 0.02
FSAWF84 Brown Crab 0.071 0.13 < 0.02
Maximum levels set out in Commission Regulation (EU) 2023/915 0.5 0.5 0.5
Dublin Bay Prawns
Sample number Species Mercury (mg/kg) Cadmium (mg/kg) Lead
(mg/kg)
FSAWF64 Dublin Bay Prawns 0.099 0.037 < 0.02
FSAWF65 Dublin Bay Prawns 0.057 0.009 0.03
FSAWF67 Dublin Bay Prawns 0.14 0.010 0.03
FSAWF68 Dublin Bay Prawns 0.065 0.007 0.03
FSAWF70 Dublin Bay Prawns 0.15 0.012 0.03
FSAWF73 Dublin Bay Prawns 0.27 0.008 0.02
FSAWF81 Dublin Bay Prawns 0.082 0.009 0.05
FSAWF82 Dublin Bay Prawns 0.15 0.011 0.06
Maximum levels set out in Commission Regulation (EU) 2023/915 0.5 0.5 0.5
Haddock
Sample number Species Mercury (mg/kg) Cadmium (mg/kg) Lead
(mg/kg)
FSAWF96 Haddock 0.098 < 0.005 < 0.02
Maximum levels set out in Commission Regulation (EU) 2023/915 0.5 0.05 0.3
Herring
Sample number Species Mercury (mg/kg) Cadmium (mg/kg) Lead
(mg/kg)
FSAWF87 Herring 0.034 < 0.005 < 0.02
FSAWF88 Herring 0.035 < 0.005 < 0.02
FSAWF89 Herring 0.042 < 0.005 < 0.02
FSAWF94 Herring 0.035 < 0.005 < 0.02
FSAWF97 Herring 0.046 < 0.005 < 0.02
FSAWF99 Herring 0.060 < 0.005 < 0.02
FSAWF100 Herring 0.034 < 0.005 < 0.02
FSAWF101 Herring 0.054 < 0.005 < 0.02
FSAWF102 Herring 0.032 < 0.005 < 0.02
FSAWF103 Herring 0.031 < 0.005 < 0.02
FSAWF104 Herring 0.052 0.006 < 0.02
FSAWF105 Herring 0.045 0.010 0.02
FSAWF106 Herring 0.040 0.006 < 0.02
FSAWF107 Herring 0.039 < 0.005 0.03
FSAWF108 Herring 0.027 0.006 < 0.02
FSAWF110 Herring 0.062 0.007 < 0.02
FSAWF111 Herring 0.047 < 0.005 < 0.02
Maximum levels set out in Commission Regulation (EU) 2023/915 0.3 0.05 0.3
King scallop
Sample number Species Mercury (mg/kg) Cadmium (mg/kg) Lead
(mg/kg)
FSAWF61 King scallop 0.008 0.28 0.07
FSAWF62 King scallop 0.012 0.40 0.10
FSAWF86 King scallop 0.009 0.24 0.16
FSAWF92 King scallop 0.010 0.33 0.09
Maximum levels set out in Commission Regulation (EU) 2023/915 0.5 1.0 1.5
Mackerel
Sample number Species Mercury (mg/kg) Cadmium (mg/kg) Lead
(mg/kg)
FSAWF90 Mackerel 0.035 < 0.005 < 0.02
FSAWF91 Mackerel 0.037 < 0.005 < 0.02
FSAWF98 Mackerel 0.030 < 0.005 < 0.02
FSAWF115 Mackerel 0.029 0.007 < 0.02
FSAWF116 Mackerel 0.043 0.013 < 0.02
FSAWF117 Mackerel 0.040 0.009 0.03
FSAWF118 Mackerel 0.040 0.014 < 0.02
Maximum levels set out in Commission Regulation (EU) 2023/915 0.3 0.1 0.3

Table 2. Dioxin/PCB WHO-TEQ 2005 and Sum ICES6 Marker PCB results for wild caught fishery products and crustaceans samples corrected for recovery.

Brown crab
Sample number Species PCDD/F WHO-TEQ upper, ng/kg whole PCB WHO-TEQ upper, ng/kg whole PCDD/F + PCB WHO-TEQ upper, ng/kg whole SUM of ICES 6 upper, µg/kg whole
FSAWF71 Brown Crab 0.145 0.0285 0.174 0.322
FSAWF85 Brown Crab 0.147 0.0461 0.193 0.230
Maximum levels set out in Commission Regulation (EU) 2023/915 3.5 6.5 75
Dublin Bay Prawns
Sample number Species PCDD/F WHO-TEQ upper, ng/kg whole PCB WHO-TEQ upper, ng/kg whole PCDD/F + PCB WHO-TEQ upper, ng/kg whole SUM of ICES 6 upper, µg/kg whole
FSAWF66 Dublin Bay Prawns 0.117 0.0580 0.175 0.305
FSAWF69 Dublin Bay Prawns 0.147 0.0776 0.225 0.568
FSAWF72 Dublin Bay Prawns 0.0792 0.0279 0.107 0.154
Maximum levels set out in Commission Regulation (EU) 2023/915 3.5 6.5 75
Haddock
Sample number Species PCDD/F WHO-TEQ upper, ng/kg whole PCB WHO-TEQ upper, ng/kg whole PCDD/F + PCB WHO-TEQ upper, ng/kg whole SUM of ICES 6 upper, µg/kg whole
FSAWF112 Haddock 0.0207 0.0105 0.0312 0.0641
Maximum levels set out in Commission Regulation (EU) 2023/915 3.5 6.5 75
Herring
Sample number Species PCDD/F WHO-TEQ upper, ng/kg whole PCB WHO-TEQ upper, ng/kg whole PCDD/F + PCB WHO-TEQ upper, ng/kg whole SUM of ICES 6 upper, µg/kg whole
FSAWF76 Herring 0.299 0.181 0.480 4.59
FSAWF93 Herring 0.472 0.674 1.15 9.87
FSAWF109 Herring 0.113 0.117 0.230 2.31
Maximum levels set out in Commission Regulation (EU) 2023/915 3.5 6.5 75
King scallop
Sample number Species PCDD/F WHO-TEQ upper, ng/kg whole PCB WHO-TEQ upper, ng/kg whole PCDD/F + PCB WHO-TEQ upper, ng/kg whole SUM of ICES 6 upper, µg/kg whole
FSAWF63 King scallop 0.0600 0.0291 0.0891 0.449
Maximum levels set out in Commission Regulation (EU) 2023/915 3.5 6.5 75
Mackerel
Sample number Species PCDD/F WHO-TEQ upper, ng/kg whole PCB WHO-TEQ upper, ng/kg whole PCDD/F + PCB WHO-TEQ upper, ng/kg whole SUM of ICES 6 upper, µg/kg whole
FSAWF74 Mackerel 0.202 0.168 0.370 3.97
FSAWF95 Mackerel 0.607 0.776 1.38 8.85
FSAWF113 Mackerel 0.102 0.238 0.340 3.72
FSAWF114 Mackerel 0.130 0.357 0.488 4.07
FSAWF119 Mackerel 0.167 0.421 0.588 3.81
Maximum levels set out in Commission Regulation (EU) 2023/915 3.5 6.5 75