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1. Dioxinand PCBs in four
commercially important
pelagic fish stocks in the
North EastAtlantic
April 2003
A project financed by Nordisk Atlantsamarbejde (NORA) together
with the Icelandic Association of Fishmeal Manufacturers and
p/f Havsbrún Faroe Islands.
2.
3. Dioxin and PCBs in pelagic fish stocks
1 Executive summary............................................................................2
2 Introduction ........................................................................................3
3 Background.........................................................................................4
3.1 Dioxin and PCBs .......................................................................4
3.2 Fishmeal and oil production in Iceland and the Faroes.............6
4 Methods and materials ......................................................................7
4.1 Sampling procedures .................................................................8
4.2 Sample handling ........................................................................9
4.3 Chemical analyses ...................................................................10
5 Results................................................................................................12
5.1 Capelin.....................................................................................22
5.2 Blue Whiting............................................................................24
5.3 Iceland Herring........................................................................26
5.4 Atlanto-Scandian Herring........................................................28
5.5 Age division of Blue Whiting..................................................31
5.6 Ratio of WHO-PCB : dioxin ..................................................34
6 Discussion..........................................................................................35
7 Acknowledgements...........................................................................37
8 References .........................................................................................38
9 Appendix 1 ........................................................................................39
10 Appendix 2........................................................................................51
11 Appendix 3........................................................................................53
1
4. Dioxin and PCBs in pelagic fish stocks
1 Executive summary
Fishmeal and fish oil of European origin have been especially criticised in a report of
the EU Scientific Committee on Animal Nutrition (SCAN) published in November
2000. Quote “Fishmeal and fish oil are the most heavily contaminated feed materials”
with respect to dioxins. The report indicated “the greatest concerns arise from the use
of fishmeals and fish oils of European origin”.
The EU Directive 2001/102/EC dated November 2001, on undesirable substances and
products in animal nutrition, specifies maximum limits for dibenzo-p-dioxins and
dibenzofurans. These compounds are commonly called dioxin.
This Directive established a maximum permissible level for dioxin of 1,25 ng WHO-
TEQ per kilogram fishmeal , and 6.00 ng WHO-TEQ per kilogram fish oil. These
limits entered into force on 1.July 2002.
The fishmeal and fish oil producers of Iceland and the Faroe Islands applied for a
grant from the Nordisk Atlantsamarbejde (NORA) in March 2000 for the finance of
an assignment with the objective to systematically collect information on dioxin as
well as polychlorinated biphenyls (PCB), in samples of landed pelagic catches and the
fishmeal and fish oil produced from each catch. This report presents the results of the
sampling that commenced in January 2001 and was completed in December 2002.
In total, 96 samples were analysed for dioxin and PCB content, from four important
fish stocks of the N.E Atlantic; capelin, blue whiting, Icelandic summer spawning
herring and Atlanto-Scandian spring spawning herring.
The results demonstrate that most of the raw material is suitable for production of
fishmeal and fish oil showing dioxin levels well below the EU limits. All of the
fishmeal produced from these 4 fish stocks is within the given maximum limit for
dioxin of 1,25ng WHO-TEQ per kg fishmeal. Based on the production figures of the
past 3 years in Iceland and the Faroes, it is estimated that more than 85% of the fish
oil production in these countries would have been below the permissible maximum
level for dioxin of 6 ng WHO-TEQ per kg fishoil.
2
5. Dioxin and PCBs in pelagic fish stocks
2 Introduction
In November 2001, the European Commission (EC) published the Directive
2001/102/EC (1) amending Directive 1999/29/EC (2) on undesirable substances and
products in animal nutrition where maximum limits on dibenzo-p-dioxin and
dibenzofuran were stipulated for feedingstuffs. These maximum limits entered into
force on 1 July 2002. The aim is to provide protective measures at the feed level with
a view to protecting public health from the possible accumulative effects of dibenzo-
p-dioxin and dibenzofuran. Parallel measures were also taken to set maximum levels
for dioxin in foodstuffs in Regulation 2375/2001 (3).
The Directive was the culmination of a scientific and political debate that had taken
place since the Belgium Incident in 1999. The opinion of the Scientific Committee on
Animal Nutrition published in November 2000 concluded that “fishmeal and fish oil
are the most heavily contaminated feed materials” with respect to dioxins. The report
indicated, “the greatest concerns arise from the use of fishmeals and fish oils of
European origin”. It also pointed out that “limited data were available on the
contamination of feed materials by WHO-PCB’s”, and suggested “scientific
cooperation should be promoted in order to collect and collate information available
in the different Member States at the EU level”(4).
As a result of this discussion, the fishmeal and fish oil producers of Iceland and the
Faroe Islands applied for a grant from the Nordisk Atlantsamarbejde (NORA) in
March 2000 for the finance of an assignment with the objective to systematically
collect information on dioxin and PCB’s in samples of landed pelagic catches and the
fishmeal and fish oil produced from each catch. This report presents the results of the
sampling that commenced in January 2001 and was completed in December 2002.
The steering committee comprised:
Derek Mundell, SR-mjöl hf. Reykjavík, Iceland (project leader)
Magnus Pauli Magnussen, Food and Environmental Agency, Tórshavn, Faroe Islands
Jón Reynir Magnusson, Association of Icelandic Fishmeal Producers, Reykjavík,
Gudny Vang, pf Havsbrún, Fuglafjörður, Faroe Islands
3
6. Dioxin and PCBs in pelagic fish stocks
3 Background
3.1 Dioxin and PCBs
The scope of this study covers the polychlorinated dibenzodioxin (PCDD) commonly
known as dioxin, polychlorinated dibenzofuran (PCDF) commonly known as furan,
and polychlorinated biphenyls (PCB). In order to simplify, this report will use the
term “dioxin” to refer to both dibenzodioxin and dibenzofuran. There are 75 possible
PCDD congeners and 135 possible PCDF congeners giving a total of 210 congeners.
Of these, 17 have been shown to be toxic, 7 PCDDs and 10 PCDFs. There are 209
possible PCB congeners of which 12 have been shown to have dioxin-like toxicity. In
order to simplify, this report will use the term “WHO-PCB” to refer to these 12 PCBs
with dioxin-like toxicity. Therefore altogether 29 congeners have dioxin-like toxicity
and they are the subjects of this study. In addition to these 29 toxic congeners, the 7
so-called Marker PCBs were measured in all the samples. These do not exhibit
dioxin-like toxicity, but have been previously used as indicators of PCB pollution.
All of these compounds are lipophilic and resist degradation. These characteristics
predispose them to long environmental persistence and to long-range transport. They
accumulate in lipid tissue and in carbon rich matrices such as soils and ocean
sediment. Dioxin and WHO-PCBs have similar chemical and toxic characteristics but
the sources of release are different. Dioxins are essentially unintentional by-products
in a number of chemical processes as well as almost all combustion processes. On the
other hand, PCBs are intentionally produced compounds that were manufactured for
decades until their use was banned in 1985. It is estimated that a total of 1,5 million
tonnes were produced worldwide before the ban was enforced (5). Although dioxin is
considerably more toxic than WHO-PCBs, the concentration of WHO-PCBs in the
environment is much higher than dioxin. For this reason, the total toxic effect of the
WHO-PCBs is often equal to or greater than that of dioxin.
The 29 toxic congeners each exhibit very different levels of toxicity on mammals. For
regulatory purposes, so called toxicity equivalency factors (TEF) have been
internationally agreed for risk assessment of complex mixtures of these 29 congeners.
The TEFs are based on acute toxicity values from in-vivo and in-vitro studies. This
approach is based on the fact that there is a common, receptor-mediated mechanism of
action for these compounds. It does not, however, take account of any synergistic or
antagonistic effects between the individual congeners with regard to toxicity.
Although the scientific basis cannot be considered to be flawless, the TEF approach
has been adopted as an administrative tool by many agencies and permits conversion
of quantitative analytical data for individual congeners into a single value of toxic
equivalent (TEQ). It must be realised that the TEFs are based on the present state of
knowledge and are subject to revision as new data becomes available. In 1997, at a
meeting of the World Health Organization, the WHO-TEF values were established
based on the existing knowledge (6). These factors have been used by the EU in their
legislation and the results in this report are based on these WHO-TEFs. The toxic
equivalents are therefore reported as concentration of WHO-TEQ. Table 1 lists these
values along with an outline of the nomenclature of the toxic congeners involved in
this study.
4
8. Dioxin and PCBs in pelagic fish stocks
3.2 Fishmeal and oil production in Iceland and the Faroes
During the years 2000 to 2002, an average of 1,7 million tonnes of fish was landed
annually and processed into fishmeal and fish oil in Iceland and the Faroes. In order
to provide information on the quantity of fishmeal and oil produced, average figures
for yield were used for each month and for each fish species. The following two
figures show the estimated monthly fishmeal production (figure 1) and fish oil
production (figure 2) based on the recorded average monthly catch landings and the
estimated fishmeal and oil yields.
Figure 1: Estimated fishmeal production in Iceland and the Faroe Islands, based
on average landed catches 2000 – 2002.
0
5
10
15
20
25
Jan Feb Mar Apr May Jun Jul Aug Sep Oct Nov Dec
%ofestimatedannualfishmealproduction
Capelin Blue whiting Iceland herring Atlanto-Scandian herring
Total average fishmeal
production was 317.000 tonnes
per annum
Figure 2: Estimated fish oil production in Iceland and the Faroe Islands, based
on average landed catches 2000 – 2002.
0
5
10
15
20
25
Jan Feb Mar Apr May Jun Jul Aug Sep Oct Nov Dec
%ofestimatedannualfishoilproduction
Capelin Blue whiting Iceland herring Atlanto-Scandian herring
Total average fish oil
production was 110.000
tonnes per annum.
6
9. Dioxin and PCBs in pelagic fish stocks
4 Methods and materials
The commercially important pelagic fish species of the northeast Atlantic area are:
Capelin (Mallotus villosus)
Two herring stocks (Clupea harengus)
o Icelandic summer spawning herring
o Atlanto-Scandian spring spawning herring
Blue whiting (Micromesistius poutassou)
The sampling was designed to assess the dioxin and PCB content of these 4 fish
stocks during the principal fishing seasons as well as in the fishmeal and fish oil
produced from them. It was, however, realised that it could be difficult to follow this
plan due to lack of fishing at the time when sampling should take place. The sampling
was done by government-approved inspectors both in Iceland and on the Faroe
Islands. Samples were taken only when boats were landing one fish species, and the
factory in question was processing only that same species. Mixtures of two or more
species were avoided. The landed catch in each case was rarely less than 1000 tonnes
except in the case of Icelandic herring catches where a minimum of 500 tonnes was
necessary. These precautions were required in order to be certain that the meal and oil
samples were definitely from the raw material that was being sampled.
It should be pointed out that all of the fishmeal in this project was produced by
indirect hot air drying or by steam drying.
Samples were taken as shown in table 2.
Table 2: Number and type of samples on a monthly basis.
Jan Feb Mar Apr May Jun Jul Aug Sep Oct Nov Dec
Capelin fish 2 2 2 4 5
fishmeal 2 2 2 4 3
fish oil 2 2 2 4 3
Iceland Herring fish 1 3 3
fishmeal 1 1 1
fish oil 1 1 1
Atl.-Scan. Herring fish 2 2 1
fishmeal 2 2
fish oil 2 2
Blue Whiting fish 2 1 1 1 1 2 2
fishmeal 2 1 1 1 1 2 2
fish oil 2 1 1 1 1 2 1
In some cases, only raw material samples were taken. There were two reasons for this
deviation from the initial plan. Firstly, the catches of capelin in the autumn months
were rather small during both years of the project. Five samples of capelin were taken
during December 2001 and December 2002; thereof 3 sets complete with fishmeal
and fish oil samples. The remaining two catches were too small (<500 mt) to justify
sampling of the fishmeal and fish oil. Secondly, the herring catches were generally
sorted according to size at landing, and the larger fish processed for human
consumption. The smaller fish and the offcuts were processed into fishmeal and oil.
7
10. Dioxin and PCBs in pelagic fish stocks
This meant that sampling of the fishmeal and fish oil would not have been
representative of the total catch. Nevertheless, it was possible to take 7 sets of herring
samples out of the 12 catches which were sampled.
This made a total of 96 samples that were taken during 2001 and 2002 depending on
the availability of the fish stocks. In 29 cases the samples were taken from the same
material as it passed through the processing system so that the fishmeal and fish oil
was directly comparable with the raw fish.
In addition to these samples, on two separate occasions during the landing of blue
whiting in the Faroe Islands, randomly taken raw fish samples were divided into three
groups of 25 fish according to size and subsequently investigated in order to provide
an insight into the effect of fish age on dioxin and WHO-PCB levels in blue whiting.
4.1 Sampling procedures
Raw material: Only whole and undamaged fish were included in the sample.
The size of the sample was as follows.
Number of individual fish
Capelin 100-110
Herring 30 - 40
Blue Whiting 100-110
Each catch was sampled throughout the landing in order to give a representative
sample of the whole load. At all stages of sample collection it was essential to avoid
contact of the sample with plastic, rubber, mineral oil and grease. All containers were
thoroughly cleaned with appropriate solvents before use in order to prevent
contamination of the samples. After sampling in Iceland, the fish were frozen as soon
as possible to prevent deterioration. In the Faroe Islands, the measuring of biological
parameters and collecting of otoliths for age determination was performed on the
fresh fish.
Fish meal: Sampling of the meal commenced when it was certain that meal
from the catch which had been sampled, had started to emerge from the production
line. A 50 –100g. meal sample was taken after the meal cooler at one hour intervals
while it was certain that the meal was still from the catch under investigation. To
prevent contamination of the sample, all contact with plastic, rubber, mineral oil and
grease was avoided.
At the end of the sampling period, the collective sample was mixed well prior to
taking two subsamples which were placed in glass containers that had been
thoroughly cleaned. Aluminium foil was placed between the container and the lid so
that the sample did not touch the lid’s lining.
Fish oil: Sampling of the fish oil from the final centrifuge commenced when it
was certain that oil from the catch which was sampled, had started to emerge from the
final centrifuge. A 100ml. fish oil sample was taken at the outlet from the centrifuge
8
11. Dioxin and PCBs in pelagic fish stocks
at one hour intervals while it was certain that the oil was still from the catch under
investigation. To prevent contamination of the sample, all contact with plastic, rubber,
mineral oil and grease was avoided.
At the end of the sampling period, the collective sample was mixed well prior to
taking three subsamples which placed in the glass containers that had been thoroughly
cleaned. Aluminium foil was placed between the container and the lid so that the
sample did not touch the lid’s lining.
4.2 Sample handling
In Iceland, when all 3 samples in a set (i.e. 1 fish sample, 1 fishmeal sample and 1 fish
oil sample) had been collected, they were sent to the Icelandic Fisheries Laboratories
(IFL) in Reykjavík.
On the Faroe Islands, a technician from the Faroese Fisheries Laboratory (FFL)
registered all the biological parameters and collected the otoliths from the fresh fish
immediately after landing at the Havsbrún plant. The otoliths were subsequently
labelled and sent to FFL in Tórshavn for age determination.
The samples were accompanied by the following information on the catch.
Fish species
Name and number of vessel
Date of catch
Area of catch
Port of landing
Size of catch
Processing plant
Date of sampling
At IFL, Reykjavík and at the Havsbrún laboratory in the Faroes, each sample was
identified with a serial number as follows:
Raw material – Iceland RM/IS -1, RM/IS -2 etc
Fishmeal – Iceland FM/IS -1, FM/IS -2 etc
Fishoil – Iceland FO/IS -1, FO/IS -2 etc
Raw material – Faroes RM/FO -1, RM/FO -2 etc
Fishmeal – Faroes FM/FO -1, FM/FO -2 etc
Fishoil – Faroes FO/FO -1, FO/FO -2 etc
Raw material. In Iceland, after thawing out the raw material samples, the fish
were individually weighed, measured for length and in the case of capelin and blue
whiting, their sex was determined. In order to determine the sex of herring, it would
have been necessary to open the abdomen. It was decided not to do this since it would
possibly have had an effect on the composition of the fish that were subsequently
homogenised and analysed. Samples were taken for age assessment (otholith sample
for blue whiting and capelin. Scale sample for herring). All care was taken not to
9
12. Dioxin and PCBs in pelagic fish stocks
damage nor contaminate the fish in this process of measurement. Immediately after
the tissue samples had been taken, the fish was coarsely minced and a portion was
homogenized as finely as possible before it was placed in a glass container with
aluminium foil inside the lid. The container was then labelled with the allocated
sample code number e.g. RM/IS – 1.
On the Faroe Islands, an official from the Faroese Fisheries Laboratory prepared the
samples in a similar way as in Iceland immediately after the biological parameters had
been measured and the otoliths removed as described previously.
On two occasions on the Faroe Islands, an additional blue whiting sample was taken
and divided into 3 groups of 25 fish. Each fish was then weighed, measured for
length, the sex was determined and then the otholiths removed for age determination.
Each group was then homogenised separately before it was placed in a glass
container. These samples were labelled RM-A/FO -# (smallest fish), RM-B/FO-#
(medium sized fish) and RM-C/FO-# (largest fish).
Fish meal: Each meal sample, as received from the factory inspector, was
labelled with the allocated serial number e.g. FM/IS -1.
Fish oil: Each oil sample as received from the factory inspector, was labelled
with the allocated serial number e.g. FO/IS –1.
All samples were deep frozen before being sent for dioxin and PCB analysis.
4.3 Chemical analyses
Fat: IFL measured fat in all raw material samples and fishmeal samples using
extraction with petroleum ether (7).
Moisture: IFL measured moisture in all raw material samples and fishmeal samples
using oven drying at 105°C (8).
Dioxin and PCBs: The steering committee selected the laboratory ERGO
Forschungsgesellschaft mbH in Hamburg to perform these analysis. This laboratory
has taken part in international interlaboratory quality control studies, organized by
WHO and EU. ERGO is regarded as one of the laboratories most experienced in this
type of analysis and has worked with the European fishmeal and fish oil industry for
several years. ERGO’s experience of the fish matrices involved in this project, has
proved to be important to the credibility of the results.
The measurements were made by high resolution gas chromatography together with
high resolution mass spectrometry (HRGC/HRMS). Prior to extraction, 13
C-UL-
labelled internal standards were added to the sample as listed in tables 3 and 4. After
spiking, the samples were extracted with nanograde solvents for ultratrace-analyses by
using a solid / lipid extraction. The extract was cleaned up on a multicolumn system
10
13. Dioxin and PCBs in pelagic fish stocks
involving carbon-on-glassfibre. The measurement was then made by means of high-
resolution gas chromatography and high-resolution mass spectrometry
(HRGC/HRMS) with VG-AutoSpec and/or Finnigan MAT 95 XL using DB-5
capillary columns.
Two isotope masses were measured for each component. The quantification was
carried out by the use of internal/external standard mixtures (isotope dilution method).
Table 3: Internal standards (13
C-UL), PCDDs/PCDFs
PCDDs PCDFs
2,3,7,8 -Tetra-CDD 2,3,7,8 -Tetra-CDF
1,2,3,7,8 -Penta-CDD 1,2,3,7,8
2,3,4,7,8
-Penta-CDF
-Penta-CDF
1,2,3,4,7,8
1,2,3,6,7,8
1,2,3,7,8,9
-Hexa-CDD
-Hexa-CDD
-Hexa-CDD
1,2,3,4,7,8
1,2,3,6,7,8
1,2,3,7,8,9
2,3,4,6,7,8
-Hexa-CDF
-Hexa-CDF
-Hexa-CDF
-Hexa-CDF
1,2,3,4,6,7,8 -Hepta-CDD 1,2,3,4,6,7,8
1,2,3,4,7,8,9
-Hepta-CDF
-Hepta-CDF
1,2,3,4,6,7,8,9 -Octa-CDD 1,2,3,4,6,7,8,9 -Octa-CDF
Table 4: Internal standards (13
C-UL), WHO-PCB
Compound IUPAC Code
3,3´,4,4´ -Tetra-CB PCB 77
3,4,4´,5 -Tetra-CB PCB 81
3,3´,4,4´,5 -Penta-CB PCB 126
Non-
ortho
PCBs
3,3´,4,4´,5,5´ -Hexa-CB PCB 169
2,3,3´,4,4´ -Penta-CB PCB 105
2,3,4,4´,5 -Penta-CB PCB 114
2,3´,4,4´,5 -Penta-CB PCB 118
2´,3,4,4´,5 -Penta-CB PCB 123
2,3,3´,4,4´,5 -Hexa-CB PCB 156
2,3,3´,4,4´,5´ -Hexa-CB PCB 157
2,3´,4,4´,5,5´ -Hexa-CB PCB 167
Mono-orthoPCBs
2,3,3´,4,4´,5,5´ -Hepta-CB PCB 189
Compound IUPAC Code
2,4,4' -Tri-PCB PCB-28
2,2',5,5' -Tetra-PCB PCB-52
2,2',4,5,5' -Penta-PCB PCB-101
2,2',3,4,4',5' -Hexa-PCB PCB 138
2,2',4,4',5,5'´ -Hexa-PCB PCB 153
MarkerPCBs
2,2',3,4,4',5,5' -Hepta-PCB PCB 180
11
14. Dioxin and PCBs in pelagic fish stocks
5 Results
The results of these analyses are summarised in table 5 (capelin), table 6 (blue
whiting), table 7 (Iceland herring) and table 8 (Atlanto-Scandian herring). All results
are presented as upperbound1
values on a lipid basis in order to make it easier to
compare raw material with the fishmeal and oil produced. In these tables the notation
N/A means “not available”.
For fishmeal and fish oil, the results are also expressed on a sample basis related to a
feedingstuff with 12% moisture. This is presented in table 9 (capelin), table 10 (blue
whiting), table 11 (Iceland herring) and table 12 (Atlanto-Scandian herring). This
method of presentation is based on the requirement as stated in the EU Directive
2001/102/EC (1). On this basis, the Directive specifies that the maximum permissible
limits are as follows:
Fishmeal 1,25 ng WHO-TEQ per kg fishmeal
Fish oil 6,00 ng WHO-TEQ per kg fish oil
The results in these three tables are presented as upperbound, lowerbound2
and
mediumbound3
values as required by the EU Directive 2002/70/EC (9) dated 26.July
2002.
The congener results in full can be found in appendix 1 on pages 39 - 50. The TEQ
figures are expressed as upperbound values and the results in brackets indicate the
limit of detection when the congener could not be detected.
These tables in appendix 1 also include the results for the 7 marker PCBs that are used
as a possible predictive tool in multivariate analysis reported in appendix 3.
The summary of the results of the age division in the two separate landings of blue
whiting, are presented in table 13. The details of the congener analyses for these two
samples are presented separately in appendix 2 on page 51 – 52.
1
Upperbound values are calculated by using the limit of quantification for the contribution of each
non-quantified congener to the TEQ.
2
Lowerbound values are calculated by using zero for the contribution of each non quantified congener
to the TEQ.
3
Mediumbound values are calculated by using half of the limit of quantification for the contribution of
each non-quantified congener to the TEQ.
12
15. Dioxin and PCBs in pelagic fish stocks
Figure 3: A map of the NE Atlantic showing the approximate position of the
catches.
The numbers refer to the sample numbers as described in the sample handling, and as
used in the following tables.
13
24. Dioxin and PCBs in pelagic fish stocks
It is not the intention of this report to analyse all of these results statistically. A
multivariate analysis was made, however, to find the best regressions within the
available data. This work was done by Gudny Vang (p/f Havsbrún, Faroe Islands) and
is presented in Appendix 3 on pages 53 - 57
The main purpose of the project was to collect data systematically in order to provide
a solid base for future discussion on the subject of dioxin and PCBs in the fishmeal
and fish oil produced from the four fish stocks under examination.
The Steering Group would, however, like to draw the reader’s attention to the
following trends and supports its observations by the use of graphs and histograms.
5.1 Capelin
During the past 30 years, capelin has been the most important pelagic stock fished in
the area of the NE Atlantic, and has been utilised for fishmeal and fish oil production.
The stock lives in the waters off the north of Iceland as far as Jan Mayen and to the
East Greenland coast. Capelin becomes sexually mature at about one year of age and
usually spawns at the end of their third year. The fish die after the spawning has taken
place in March or April (10).
The average annual capelin landings in Iceland and the Faroes amounted to a total of
1.075.000 tonnes during the past 3 years (2000 – 2002). Capelin has comprised about
64% of the catch landed for meal and oil production in these two countries, and has
provided approximately 60% of fishmeal and 67% of fish oil produced there.
Figure 4: Concentration of dioxin in all capelin samples, expressed on a lipid
basis, together with the variation in fat level in the raw fish samples.
0
1
2
3
4
5
6
10.01.01
26.01.01
05.02.01
27.02.01
05.03.01
22.03.01
04.07.01
11.07.01
23.07.02
24.07.01
03.12.02
09.12.02
10.12.01
10.12.02
17.12.01
Dioxin
ngWHO-TEQ/kglipid
0
2
4
6
8
10
12
14
16
18
Fishfat%
Raw material Fish meal Fish oil Fish fat %
A
B
Fat content and roe content are closely related to the capelin’s lifecycle. The fat
content starts to increase during the third year of the lifespan usually reaching a
22
25. Dioxin and PCBs in pelagic fish stocks
maximum of 15 – 16% fat in October / November (section marked “B” on figures 4
and 5). During the following 3 months, the reproductive organs increase rapidly in
size and the fish cease feeding. Therefore the body fat content drops rapidly during
the period from late December until spawning takes place in March or early April
when the fat level has dropped to 3% (section marked “A” on figures 4 and 5). On
average during the past 3 years, 80% of the capelin has been fished during the months
January to March. At that time of year the 3-year-old spawning fish is separated from
the younger fish and the catches are therefore almost entirely comprised of 3-year-old
fish.
Since dioxin and PCBs are lipophilic and persistant, then when the fat level of the fish
decreases rapidly as it does in the capelin during the last months of its life, it can be
expected that dioxin and PCBs would become more concentrated in the lipid phase.
This is reflected in the capelin results for January, February and March when the
concentration of these compounds shows a steady increase in the lipid phase (Figure 4
dioxin and figure 5 WHO-PCB).
Figure 5: Concentration of WHO-PCBs in all capelin samples, expressed on a
lipid basis, together with the variation in fat level in the raw fish
samples.
0
1
2
3
4
5
6
7
8
9
10.01.0126.01.0105.02.0127.02.0105.03.0122.03.01
04.07.0111.07.0123.07.0224.07.0103.12.0209.12.0210.12.0110.12.0217.12.01
WHO-PCB
ngWHO-TEQ/kglipid
0
2
4
6
8
10
12
14
16
18
Fishfat%
Raw material Fish meal Fish oil Fish fat %
A
B
During the summer capelin season in July, the 2-year-old fish is feeding and gradually
becoming fatter. The fat level in July is normally about 11% and increases to about
16% in November as mentioned earlier. This means that dioxin and WHO-PCB levels
in July are even lower than those in the winter-capelin (figures 4 and 5).
On average, the level of WHO-PCB in the lipid phase of capelin is 70% higher than
the dioxin level.
The results for the dioxin concentration in fishmeal and fish oil were also expressed
on a sample basis assuming 12% moisture content. In figure 6 these results are
23
26. Dioxin and PCBs in pelagic fish stocks
compared to the maximum permissible levels for dioxin in fishmeal and fish oil as
stated in the EU Directive.
Figure 6: Concentration of dioxin in all capelin-meal and -oil samples, expressed
on a sample basis assuming 12% moisture.
0
1
2
3
4
5
6
7
10.01.01 26.01.01 05.02.01 27.02.01 05.03.01 22.03.01 04.07.01 11.07.01 23.07.02 24.07.01 03.12.02 09.12.02 10.12.01
DioxinngWHO-TEQ/kgsample
Fish meal Fish oil Limit fish meal Limit fish oil
5.2 Blue Whiting
Blue whiting is a migratory stock living in the Atlantic waters from Portugal and
north to the Barents Sea. It consists of several stocks but is treated by ICES as one
stock since it has not been possible to define clear divisions between populations. It
has been fished by EU, Norway and Russia as well as Iceland and the Faroes (11).
The average annual blue whiting landings in Iceland and the Faroes amounted to a
total of 474.000 tonnes during the past 3 years (2000 – 2002). Blue whiting has
comprised about 28% of the catch landed for meal and oil production in these two
countries, and has provided approximately 30% of fishmeal and 16% of fish oil
production.
Blue whiting spawn mostly in an area to the west of Scotland and Ireland in March –
April, although there are other spawning areas off Portugal, the Faroe Islands, SW
Iceland and in the Norwegian fjords. The fish can reach sexual maturity between 2-7
years old and can live for up to 20 years (10).
This fish stores most of its fat reserves in the liver. The fat level of whole fish can
vary from 1% in April / May directly after spawning, up to 8% during the winter
months. It would seem that dioxin and WHO-PCB levels in the lipid phase vary
inversely with the fat level in the fish (figure 7 dioxin and figure 8 WHO-PCB).
24
27. Dioxin and PCBs in pelagic fish stocks
Figure 7: Concentration of dioxin in all blue whiting samples, expressed on a
lipid basis, together with the variation in fat level in the raw fish
samples.
0,0
5,0
10,0
15,0
20,0
25,0
10.02.01 24.02.01 18.03.01 18.04.01 05.05.01 20.08.01 06.09.01 15.09.01 14.11.01 15.11.01
Dioxin
ngWHO-TEQ/kglipid
0
2
4
6
8
10
12
Fishfat%
Raw material Fish meal Fish oil Fish fat %
Figure 8: Concentration of WHO-PCBs in all blue whiting samples, expressed on
a lipid basis, together with the variation in fat level in the raw fish
samples.
0
10
20
30
40
50
60
70
80
90
10.02.01 24.02.01 18.03.01 18.04.01 05.05.01 20.08.01 06.09.01 15.09.01 14.11.01 15.11.01
WHO-PCB
ngWHO-TEQ/kglipid
0
2
4
6
8
10
12
Fishfat%
Raw material Fish meal Fish oil Fish fat %
Levels of these compounds in the whole fish fat is highest in April / May and lowest
from September to November.
25
28. Dioxin and PCBs in pelagic fish stocks
On average, the level of WHO-PCB in the lipid phase of blue whiting is 265% higher
than the dioxin level.
The results for the dioxin concentration in fishmeal and fish oil were also expressed
on a sample basis assuming 12% moisture content. In figure 9 these results are
compared to the maximum permissible levels for dioxin in fishmeal and fish oil as
stated in the EU Directive.
Figure 9: Concentration of dioxin in all blue whiting-meal and -oil samples,
expressed on a sample basis assuming 12% moisture.
0
2
4
6
8
10
12
14
16
10.02.01 24.02.01 18.03.01 18.04.01 05.05.01 20.08.01 06.09.01 15.09.01 14.11.01 15.11.01
DioxinngWHO-TEQ/kgsample
Fish meal Fish oil Limit fish meal Limit fish oil
5.3 Iceland Herring
The Icelandic spring spawning herring lives in coastal waters around Iceland and has
been utilised since the mid 1970’s. The stock spawns in July off the SW and SE of
Iceland and then migrates in search of feeding grounds off the west and east coasts.
This herring stock becomes sexually mature at about 4 years of age and can live for
20 – 25 years (10). The catch is seasonal, mostly taking place in October to January off
the east, south and west coasts of Iceland.
The average annual landings of Icelandic herring in Iceland, which were used for
fishmeal and fish oil production, amounted to a total of 40.000 tonnes during the past
3 years (2000 – 2002). Icelandic herring has comprised about 3% of the catch landed
for meal and oil production, and has provided approximately 3% of fishmeal and 6%
of fish oil production. These figures can be variable depending on the proportion of
the total catch that is processed for human consumption.
The average age of the catches in this study ranged from 3 to 9 years, which can be
considered quite normal for this stock. The fat content of whole fish during the fishing
season (September – January) is fairly stable at about 16% and does therefore not
26
29. Dioxin and PCBs in pelagic fish stocks
have an influence on dioxin and WHO-PCB levels. (figure 10 dioxin and figure 11
WHO-PCB).
Figure 10: Concentration of dioxin in all Iceland herring samples, expressed on
a lipid basis, together with the variation in fat level in the raw fish
samples.
0
1
2
3
4
5
6
28.10.02 16.11.02 26.11.01 28.11.01 02.12.02 04.12.02 09.12.02
Dioxin
ngWHO-TEQ/kglipid
0
2
4
6
8
10
12
14
16
18
20
Fishfat%
Raw material Fish meal Fish oil Fish fat %
Figure 11: Concentration of WHO PCBs in all Iceland herring samples,
expressed on a lipid basis, together with the variation in fat level in the
raw fish samples.
0
1
2
3
4
5
6
7
8
9
28.10.02 16.11.02 26.11.01 28.11.01 02.12.02 04.12.02 09.12.02
WHO-PCB
ngWHO-TEQ/kglipid
0
2
4
6
8
10
12
14
16
18
20
Fishfat%
Raw material Fish meal Fish oil Fish fat %
27
30. Dioxin and PCBs in pelagic fish stocks
On average, the level of WHO-PCB in the lipid phase of Icelandic herring is 100%
higher than the dioxin level.
The results for the dioxin concentration in fishmeal and fish oil were also expressed
on a sample basis assuming 12% moisture content. In figure 12 these results are
compared to the maximum permissible levels for dioxin in fishmeal and fish oil as
stated in the EU Directive.
Figure 12: Concentration of dioxin in all Iceland herring-meal and -oil samples,
expressed on a sample basis assuming 12% moisture.
0
1
2
3
4
5
6
7
28.10.02 16.11.02 02.12.02
DioxinngWHO-TEQ/kgsample
Fish meal Fish oil Limit fish meal Limit fish oil
5.4 Atlanto-Scandian Herring
The Atlanto-Scandian herring stock (spring spawning herring) is found in the open
seas of the northeast Atlantic. This stock spawns in February to April off western
Norway, and the immature fish stay in Norwegian waters while the adult fish migrate
in search of feed further out into the northeast Atlantic. (10)
The average annual landings of Atlanto-Scandian herring in Iceland that were used for
fishmeal and fish oil production, amounted to a total of 100.000 tonnes during the past
3 years (2000 – 2002). Atlanto-Scandian herring has comprised about 6% of the catch
landed for meal and oil production, and has provided approximately 7% of fishmeal
and 12% of fish oil production. These figures can be variable depending on the
proportion of the total catch that is processed for human consumption.
Fat content of whole fish during the months of fishing (May – September) can be very
variable depending on the proportions of immature fish (high in fat) and newly
spawned fish (low in fat) in the catch. Dioxin and WHO-PCB levels in the lipid phase
are therefore quite variable, both because of the effect of fat level and also the effect
of age. (figure 13, dioxin and figure 14, WHO-PCB).
28
31. Dioxin and PCBs in pelagic fish stocks
Figure 13: Concentration of dioxin in all Atlanto-Scandian herring samples,
expressed on a lipid basis, together with the variation in fat level in the
raw fish samples.
0
2
4
6
8
10
12
14
26.05.02 28.05.01 07.06.02 15.06.01 10.09.01
Dioxin
ngWHO-TEQ/kglipid
0
5
10
15
20
25
Fishfat%
Raw material Fish meal Fish oil Fish fat %
Figure 14: Concentration of WHO PCBs in all Atlanto-Scandian herring
samples, expressed on a lipid basis, together with the variation in fat
level in the raw fish samples.
0
2
4
6
8
10
12
14
16
18
20
26.05.02 28.05.01 07.06.02 15.06.01 10.09.01
WHO-PCB
ngWHO-TEQ/kglipid
0
5
10
15
20
25
Fishfat%
Raw material Fish meal Fish oil Fish fat %
On average, the level of WHO-PCB in the lipid phase of Atlanto-Scandian herring is
50% higher than the dioxin level.
The results for the dioxin concentration in fishmeal and fish oil were also expressed
on a sample basis assuming 12% moisture content. In figure 15 these results are
29
32. Dioxin and PCBs in pelagic fish stocks
compared to the maximum permissible levels for dioxin in fishmeal and fish oil as
stated in the EU Directive.
Figure 15: Concentration of dioxin in all Atlanto-Scandian herring-meal and -oil
samples, expressed on a sample basis assuming 12% moisture.
0
2
4
6
8
10
12
26.05.02 28.05.01 07.06.02 15.06.01
DioxinngWHO-TEQ/kgsample
Fish meal Fish oil Limit fish meal Limit fish oil
30
33. Dioxin and PCBs in pelagic fish stocks
5.5 Age division of Blue Whiting
Fish samples from two of the landings of blue whiting in the Faroe Islands, were
separated according to size. Despite the fact that the fish fat levels and sex ratios were
very different in these six samples, it is nevertheless apparent that the levels of dioxin
and WHO-PCB increase with age (figure 16 dioxin and figure 17 WHO-PCB).
Figure 16: Regression of dioxin concentration in the lipid against fish age.
R2
= 0,9162
0,0
5,0
10,0
15,0
20,0
25,0
0 1 2 3 4 5 6
Age (yrs)
Dioxin
ngWHO-TEQ/kglipid
Figure 17: Regression of WHO-PCB concentration in the lipid against fish age
R2
= 0,852
0
10
20
30
40
50
60
70
80
90
100
0 1 2 3 4 5
Age (yrs)
WHO-PCB
ngWHO-TEQ/kglipid
6
31
34. Dioxin and PCBs in pelagic fish stocks
Fish length (figure 18, dioxin and figure 19, WHO-PCB) and fish weight (figure 20,
dioxin and figure 21, WHO-PCB) are not as well correlated with the levels of these
compounds.
Figure 18: Regression of dioxin concentration in the lipid, against fish length.
R2
= 0,7586
0,0
5,0
10,0
15,0
20,0
25,0
10 15 20 25 30 35
Fish Length (cm)
Dioxin
ngWHO-TEQ/kglipid
Figure 19: Regression of WHO-PCB concentration in the lipid, against fish
length
R2
= 0,73
0
10
20
30
40
50
60
70
80
90
100
10 15 20 25 30 35
Fish Length (cm)
WHO-PCB
ngWHO-TEQ/kglipid
32
35. Dioxin and PCBs in pelagic fish stocks
Figure 20: Regression of dioxin concentration in the lipid, against fish weight
R
2
= 0,7603
0,0
5,0
10,0
15,0
20,0
25,0
10 30 50 70 90 110 130 150 170
Fish Weight (g)
Dioxin
ngWHO-TEQ/kglipid
Figure 21: Regression of WHO-PCB concentration in the lipid, against fish
weight.
R2
= 0,774
0
10
20
30
40
50
60
70
80
90
100
10 30 50 70 90 110 130 150 170
Fish Weight (g)
WHO-PCB
ngWHO-TEQ/kglipid
33
36. Dioxin and PCBs in pelagic fish stocks
5.6 Ratio of WHO-PCB : dioxin
The following table shows the average levels of dioxin and of WHO-PCB for the 4
fish stocks in this investigation. All types of samples were included. The upperbound
results in the lipid phase were used for this comparison as reported in tables 5, 6, 7
and 8.
Table 14: Comparison of average levels of dioxin and WHO-PCB
Dioxin WHO-PCB
ng WHO-TEQ /kg lipid
Ratio PCB /
dioxins
Number of
samples
Capelin 2,0 3,4 1,7 41
Blue Whiting 6,2 22,6 3,6 29
Iceland Herring 2,3 4,6 2,0 13
Atlanto-Scandian Herring 6,9 10,2 1,5 13
The age division samples of blue whiting show that there is a good correlation
between the ratio of WHO-PCB : dioxin when compared to age. This is shown in the
following figure 22.
Figure 22: Blue whiting age division samples. Regression of the ratio WHO-
PCB : dioxin, against age.
R2
= 0,9138
0,00
1,00
2,00
3,00
4,00
5,00
0 1 2 3 4 5 6
Age (yrs)
Ratio
WHO-PCB/Dioxin
34
37. Dioxin and PCBs in pelagic fish stocks
6 Discussion
According to the EU Directive 2002/32 (12), after 1.August 2003 it will be prohibited
within the EEA, to blend down feed materials that exceed the maximum limit for
dioxin. This will mean that fish oil which exceeds the limit for dioxin of 6 ng WHO-
TEQ per kg oil will either have to be sold for industrial use, or must be sent for
decontamination. Fishmeal exceeding the maximum limit for dioxin of 1,25 ng TEQ
per kg meal must be destroyed in a controlled manner or else be decontaminated.
The results from this project demonstrate that most of the raw material is suitable for
production of fishmeal and fish oil showing dioxin levels well below the EU limits.
All of the fishmeal produced from these 4 fish stocks is within the given maximum
limit for dioxin of 1,25ng WHO-TEQ per kg meal. Based on the production figures
of the past 3 years in Iceland and the Faroes, it is estimated that more than 85% of the
fish oil production in these countries would have been below the permissible
maximum level for dioxin of 6 ng WHO-TEQ per kg fishoil.
All capelin products were well within the given dioxin limits.
All blue whiting meal was well within the limit for fishmeal.
Blue whiting oil produced when the fish fat level is below approximately 4%, should
be kept separate from other production until it has been measured for dioxin. There is
a strong likelihood that the level of dioxin in this production is above the EU limit.
During the period 2000 – 2001, there was an average blue whiting oil production of
approximately 3000 tonnes in Iceland and the Faroes during the critical months of
March, April and May. This is less than 3% of the total fish oil production during
these 3 years.
All Icelandic herring products were well within the given dioxin limits.
All Atlanto-Scandian herring meal was well within the limit for dioxin.
Fish oil produced from Atlanto-Scandian herring was close to or above the EU
maximum limit for dioxin. The results indicate that if fish fat level in this stock goes
below 13% then the dioxin level could be close to or above the EU maximum limit.
This production should be kept separate from other fish oil until it has been measured
for dioxin. During the three years from 2000 – 2002, there was an average herring oil
production from this stock of approximately 12.000 tonnes in Iceland and the Faroes
during the months of May, June and July. This is less than 12% of the total fish oil
production during these 3 years.
It is evident that concentrations of dioxin and WHO-PCBs are inversely related to the
level of fat in the fish, but increase with the age of the fish.
The age division samples of blue whiting indicate that in this species there could be a
greater tendency to accumulate WHO-PCBs as opposed to dioxin, since the ratio of
WHO-PCB to dioxin increases with age. Although similar data are not available for
35
38. Dioxin and PCBs in pelagic fish stocks
the other fish species in this study, it would appear that this tendency is not apparent
in herring nor capelin.
In addition to fish fat level and age there are at least three other factors that could
possibly influence the relative levels of these compounds in the fish.
Migration area. The ratio of WHO-PCB compared to dioxin is variable
between fish stocks. This reflects the fact that the sources for these two groups
of compounds are very different. It can be concluded that migration area has
probably a direct effect on the levels of dioxin and WHO-PCB. Blue whiting
is a migratory fish and as such could have been living in an area of the NE
Atlantic that is very distant from the area where it is caught.
Sex ratio of the catch. Females are able to reduce their dioxin and PCB load,
each time they spawn. Evidence of this effect could not be seen in the results
of the blue whiting. Capelin spawns only once and therefore the effect cannot
be seen in that species. Sex was not determined on the herring samples as
explained previously.
Physiology. Blue whiting is a species that stores most of of its body fat in the
liver, as opposed to capelin and herring that store their fat in adipose tissue
throughout the body. This means that the blue whiting has most of the dioxin
and PCBs in the liver tissue, which is where biotransformation of such
compounds normally takes place. Further studies of the congener data in
appendix 1 could clarify whether this could be a significant contributing factor
to explain the higher WHO-PCB : dioxin ratio which is observed in the blue
whiting results. This, however, is not within the scope of the present report.
All of these five factors could be affecting the levels of dioxin and PCBs
simultaneously. The results of this investigation, however, give a much clearer idea of
the variations involved with these 4 pelagic stocks in the NE Atlantic and are most
useful in clarifying the limitations the EU directives impose on the products from
these stocks.
36
39. Dioxin and PCBs in pelagic fish stocks
7 Acknowledgements
The steering committee should like to thank the Award Committee of Nordisk
Atlantsamarbejde (NORA) for supporting this project. Without their understanding
these valuable results would not be available to the industry. In addition we should
like to thank the staff of the Icelandic Fisheries Laboratories, The Icelandic Marine
Research Institute and the Faroese Fisheries Laboratory for their professional
assistance with age determination and sample preparation. We also greatly appreciate
the coordination work done by Miss Claudia Collingro and Dr Thomas Herrmann of
ERGO with regard to the analysis and transfer of results. We should like to thank
Thorhallur Jonasson, Quality Manager of SR-mjöl hf for his help in coordinating the
sampling in Iceland. And finally we are grateful to Gudjon Atli Audunsson of IFL for
the many useful discussions regarding the results and their presentation.
37
40. Dioxin and PCBs in pelagic fish stocks
8 References
1. Council Directive 2001/102/EC of 27.November 2001 on "the undesirable
substances and products in animal nutrition”, Official Journal of the
European Communities L6, 10/01/2002 pp. 45 – 49
2. Council Directive 1999/29/EC of 27.April 1999 on “the undesirable
substances and products in animal nutrition”, Official Journal of the
European Communities L115, 04/05/1999 pp. 32 – 46
3. Council Regulation 2375/2001 of 29.November 2001 on “setting
maximum levels for certain contaminants in foodstuffs”, Official Journal
of the European Communities L321, 06/12/2001 pp. 1 – 5
4. Opinion of the Scientific Committee on Animal Nutrition on Dioxin
Contamination of Feedingstuffs and their Contribution to the
Contamination of Food of Animal Origin, 6th November 2000
5. J. Rantanen, Industrial and Environmental Emergencies; Lessons Learned.
Organohalogen Compd. 10 (1992) 291 – 294
6. Martin Van den Berg et al. Toxic Equivalency Factors (TEFs) for PCBs,
PCDDs, PCDFs for Humans and Wildlife, Environmental Health
Perspectives 106 (1997) 775 – 792
7. AOCS Official Method Ba 3-38, 1997
8. ISO 6496-1999
9. Council Directive 2000/70/EC of 26.July 2002 on “establishing
requirements for the determination of levels of dioxins and dioxin-lke
PCBs in feedingstuffs”, Official Journal of the European Communities
L209, 06/08/2002 pp. 15 – 21
10. Sjávarnytjar við Ísland (1998), Gunnarsson, K., Jónsson, G., and Pálsson,
Ó., Mál and Menning, Reykjavík
11. International Council for the Exploration of the Sea: Report nr 255 of the
ICES Advisory Committee on Fishery Management, December 2002
12. Council Directive 2002/32/EC of 7.May 2002 on “the undesirable
substances in animal feed”, Official Journal of the European Communities
L140, 30/05/2002 pp. 10 – 21
38
41. Dioxin and PCBs in pelagic fish stocks
9 Appendix 1
The congener results are presented on pages 40 – 50. The figures in brackets indicate
the limit of determination when the congener could not be detected.
These results can be provided electronically by contacting the members of the steering
committee.
Derek Mundell derek@srmjol.is
Magnus Pauli Magnussen magnuspm@hfs.fo
Jón Reynir Magnusson jr@fif.is
Gudny Vang gur@havsbrun.fo
39
