veterinær grensekontrollrapport 2012

Helge Torbjørn Hove, Bjørn Tore Lunestad, Irja Sunde Roiha and

Amund Måge

Nasjonalt institutt for ernærings- og sjømatforskning (NIFES)

04.04.2014

MONITORING PROGRAMME FOR VETERINARY CONTROL ON SEAFOOD

PRODUCTS IMPORTED TO NORWAY FROM THIRD COUNTRIES

In accordance with Commission Regulation (EC) No 136/2004, Annex II, Part 1.

RESULTS FROM 2012

2012

Rapport

Monitoring program for veterinary control on fisheries products imported to Norway from third countries, 2012.

2

Acknowledgements

This report presents a summary of the marine part of veterinary border control project which

the National Institute of Nutrition and Seafood Research (NIFES) partly carries carried out by

a mandate from the Norwegian Food Safety Authority (NFSA). NIFES participated in the

elaboration of the sampling plans and were given the responsibility to carry out the analytical

work and to elaborate this annual report. We wish to thank the NFSA for excellent

cooperation during the conduct of this monitoring programme.

Staff involved in the technical tasks for this project in 2012: Anne Margrethe Aase

administrated the day to day technical work, including sample reception, sample storage, and

aliquot preparation and distribution within NIFES. Annette Bjordal, Anette Kausland, Marita

Kristoffersen and Annbjørg Bøkevoll were in charge of the analytical work, while Manfred

Torsvik, Vidar Fauskanger and Kari Pettersen carried out the sample pre-treatment. Tone

Galluzzi, Betty Irgens and Leikny Fjeldstad were responsible for the microbiological

examinations. The examinations with respect to parasites were performed by Leikny

Fjeldstad. Tore Tjensvoll, Eva Torgilstveit and Rita Hannisdal were responsible for the

chemical analysis for residues of therapeutics. Karstein Heggstad, Tadesse T. Negash,

Jannicke A. Berntsen, Dagmar Nordgård, Lene H. Johannessen, Britt Elin Øye, Pablo Cortez,

Kari Breistein Sæle, Kjersti Pisani, Tina C. Rossvold, Joseph Malaiamaan, Betty Irgens, Thu

Thao Nguyen, Ingjerd Hauvik and Elilta Hagos were responsible for extraction, clean-up and

determination of the organic contaminants. Jorun Haugsnes, Siri Bargård, Tonja Lill Eidsvik,

Berit Solli, Edel Erdal and Laila Sedal carried out the analysis of the chemical elements.

Histamine determination was carried out by Joseph Martin Malaiamaan and Margrethe Rygg.

Total volatile basic nitrogen analysis was carried out by Georg Smith Olsen.


3

Index ......................................................................................................................................... 3

1. Abstract, summary and recommendations ..................................................................... 5

2. Terminology ....................................................................................................................... 8

3. Introduction ..................................................................................................................... 11

3.1. Background and purpose ............................................................................................... 11

3.2 The legal foundation ....................................................................................................... 11

3.3. The planning and scope of the work .............................................................................. 11

4. Materials and methods ................................................................................................... 12

4.1. Sampling ........................................................................................................................ 12

4.2. Sample reception, registration and pre-analytical sample handling .............................. 12

4.3. Chemical analytical methods and microbiological assays ............................................ 12

4.3.1 Quality assurance ..................................................................................................... 13

4.4 Other analytical methods ................................................................................................ 13

4.4.1. Method for oil authentication .................................................................................. 13

4.4.2. Analytical sub-contractor ........................................................................................ 14

4.5 Application of maximum limits to non-standard products ............................................. 14

5. Results and discussion .................................................................................................... 15

5.1. Microbiology ................................................................................................................. 15

5.2. Parasites ......................................................................................................................... 16

5.3. Drug residues and dyes .................................................................................................. 16

5.4. Chemical spoilage and rancidity indicators ................................................................... 16

5.5. Oil authentication .......................................................................................................... 17

5.6. Heavy metals ................................................................................................................. 17

5.6.1. Arsenic (As) ............................................................................................................ 17

5.6.2. Cadmium (Cd) ........................................................................................................ 17

5.6.3. Mercury (Hg) .......................................................................................................... 17

5.6.4. Lead (Pb) ................................................................................................................. 18

5.7. Persistent organic pollutants (POPS) ............................................................................. 18

Index


4

5.7.1. The dioxins; PCDDs, PCDFs and DLPCBs ........................................................... 18

5.7.2. The indicator PCBs ................................................................................................. 18

5.7.3. Polybrominated diphenyl ethers (PBDE) ................................................................ 18

5.7.4. Pesticides ................................................................................................................. 18

5.7.5. Polyaromatic hydrocarbons, PAH .......................................................................... 19

Annex 1: Data Tables ............................................................................................................. 20

Annex 2: Table 14 A summary of legal maximum limits ................................................... 47

Annex 3: Table 15 Method performance data ..................................................................... 48


5

1. Abstract, summary and recommendations

The present report summarizes the monitoring project for veterinary border control performed

on fish and other seafood imported to Norway from outside the European Economic Zone. A

risk assessment for the different imported products was the basis for the sampling plans and

activities in this program. The risk assessment was founded on the current trend of hazards as

reported in the RASSF notification system, on the compositional nature the products, on their

geographical origin as well as on the annual import quantity. On this background, the activity

in the programme was planned for commodities with the highest risk.

In 2012, 144 samples were taken according to a priority selection plan to be assayed for

chemical, biological and/or microbiological undesirables based on their hazard profiles.

Microbiological analysis was performed on 140 of the samples, and the selection of

parameters to be examined was adjusted to the product category. The results for

microbiological quality parameters and indicator organisms for faecal contamination

generally showed low bacterial counts, with some exceptions. L. monocytogenes and

pathogenic Vibrio species were not detected in any samples. Salmonella was detected in one

sample of raw, frozen scampi imported from Vietnam. The serovar of the isolate were found

to be Weltevreden.

Parasitological examinations were carried out on 60 samples of fish. Nematodes were found

in 17 samples (28% of tested samples). The highest number of nematodes was found in a fillet

sample of Greenland halibut at 32 nematodes. Parasites were also found in samples of cod,

haddock, redfish, saithe and mackerel.

Samples originating from of aquaculture were also analysed for residues of pharmaceutical

compounds and dyes. A total of 18 samples were assayed for dyes, including crystal violet,

leuco crystal violet, malachite green, leuco malachite green and brilliant green. Analysis for

chloramphenicol and nitrofuranes (including their metabolites) were also carried out on these

18 samples. No residue of dyes or drugs could be detected in these samples.

Eighteen samples were analysed for one or more of the spoilage indicators, histamine and

TVB-N or TBARS (a measure of rancidity). From a food safety point of view, the measured

values gave little reason for concern. Some values did, however, suggest that the associated

sample had been exposed to improper storage conditions before the border crossing. This is

consistent with findings from previous years.


6

A total of 109 samples were analysed for the elements cadmium, mercury, lead and arsenic.

None of the samples was found non-compliant with regard to the maximum limits for these

elements. However, a sample of squid oil from South Korea had a high level of Cd, but no

legal limit for cadmium applies to this kind of sample.

For the monitoring of persistent organic substances, (POPs) a range of compound-classes of

undesirables were analysed.

A total of 31 samples were analysed for dioxins and PCBs. The analytical levels were

transformed to TE values, “toxic equivalents”, as defined by WHO (2005). Further, four

samples were analysed for “indicator PCBs”. One sample of squid oil from South Korea

exceeded the maximum limit for the sum of total TE, with a sum-value of 41 pg TE/g. The

dioxin like PCBs were the main contributors to the high value. This was an oil sample from

Todarodes sagittatus, the European flying squid (cuttlefish). The finding is consistent with

results from previous years in that samples of this species may have high values of organic

contaminants.

Flame retardants were also measured and the PBDE class of compounds were analysed in 29

samples. Two samples were found to have analytical levels of significance. The sums of 7-

PBDE were 33 and 14 µg/kg w.w. in two samples of marine oil, one from South Korea and

one from USA.

A total of 22 samples were analysed for chlorinated pesticides. Most of these were not

detected or were found in very low levels in all samples. The levels found in seafood were

generally lower than the values found in oil. Two samples of oil, one from Korea and one

from the USA, had elevated levels of pesticides. There is no legal limit for chlorinated

pesticides in marine oils if they are used for humans. The measured value of p,p’-DDE in the

previously mentioned oil from Korea, 100 μg/kg w.w., was the highest analytical level found

of all the undesirables measured.

For the PAH class of compounds, the legislation was changed during 2012. A new upper limit

for the lower bound sum of four PAH compounds (4PAH) were set. The maximum limits for

benzo(a)pyrene (BaP) are still maintained for some foodstuffs, but not for fish fillet. One of

the 23 analysed samples was found to exceed the new limit for the 4PAH, but this was

sampled prior to the date of implementation for the regulation and was the same sample of

squid oil mentioned above.

NIFES is asked to give future recommendations on sampling and analyses in this monitoring

programme. Based on our findings over time we recommend an increased activity on the

microbiological parameters. For farmed species, we recommend an increased activity targeted

on pharmacologically active substances. A directed sampling regime for parasitological

relevant samples should further be considered.


7

NIFES further recommends that for heavy metals and POPs parameters, in response to the

change in legislation from 2012, the focus should be turned towards the parameters with new

legal limits assigned to them for the next few years. Also, the product/ country of origin

combinations with a known history of illegal levels should be focussed with a high sampling

frequency. With regard to oil authentication, an activity should be maintained at a low level of

sampling.

The chemical spoilage and rancidity parameters are not a mandatory part of this monitoring

programme. However, this monitoring has for years reviled that a low proportion of the

samples have been exposed to improper storage or transport conditions. It is well known that

a range of hazards that can develop under such conditions. The activity to monitor these

parameters should at least be kept at the present level.


8

2. Terminology

Analyte: The chemical substance that is the target for a chemical analysis.

BIP: EU and Norwegian Border Inspection Post.

CFU: Colony forming units, the number of microorganisms (bacteria or fungi) able to grow

on solid agar media giving a visible colony that can be counted.

Congener: In this context “congeners” refers to analogous compounds within the classes

PCB, PBDE, dioxins, furans and thoxaphenes. A congener is usually referred to by a unique

ID number: CB-147, PBDE-47 or Tox-62. The congeners in each class are closely related in

chemical properties. The differences between the congeners within a class are the number and

the position of the halogen atoms (chlorine or bromine) attached to an otherwise identical

molecular structure.

DLPCB: Dioxin-like PCBs. PCB congeners with non-orto and mono-orto halogen

substitution pattern in their chemical structure. Their toxicity is similar to the dioxins and

furans.

Histamine: A chemical compound responsible for “scombroid food poisoning” from eating

mackerel, tuna, bluefish, mahi-mahi, bonito, sardines, anchovies, and related species of fish

that were inadequately refrigerated or preserved. Histamine is formed from histidine, a natural

compound found in quantity in these fish species. Histamine is extremely stable once formed

and is not affected by cooking. The analytical level of histamine in fish is used as a spoilage

indicator.

ICES: The International Council for the Exploration of the Sea.

LOQ and LOD: Limit of quantification and Limit of detection: The LOD is the lower

limit for reliably to conclude on the presence/ absence of the analyte in the sample. The LOQ

is the lower limit for a reliable quantitative measurement. The internationally recognized

abbreviations LOQ and LOD are used. LOQ is normally higher than LOD by a factor of 3.0 to

3.3. For compounds that are illegal in fish the LOD is most relevant, since any detection of

the compound would be indicative of its use. For other compounds quantification is required.

Concentrations below LOQ will be reported as “less than LOQ”, for example: < 2.0 μg/kg.

Illegal compounds will on the other hand, depending on the measured concentration, be

reported as: “ND” (Not detected), “Detected”, or if it was above the LOQ as the numeric

value measured.

http://en.wikipedia.org/wiki/Scombridae

http://en.wikipedia.org/wiki/Mackerel

http://en.wikipedia.org/wiki/Tuna

http://en.wikipedia.org/wiki/Bluefish

http://en.wikipedia.org/wiki/Mahi-mahi

http://en.wikipedia.org/wiki/Bonito

http://en.wikipedia.org/wiki/Sardine

http://en.wikipedia.org/wiki/Anchovies


9

LIMS: Laboratory Information Management System: A software system in which the sample

is registered and administrated and the corresponding analytical results are registered and

stored.

Matrix: In chemical analysis matrix refers to the components of a sample other than the

analyte of interest.

Maximum residue limit (MRL): MRL is the legal maximum concentration of residue of

pharmaceuticals in a food product obtained from an animal that has received treatment of

veterinary medicine. MRL values are found in EU and Norwegian legislation.

Maximum Levels (ML): ML is set for certain contaminants in foodstuffs mainly through EU

regulations 1881/ 2006 and these has generally been adopted into the Norwegian Food Law as

well. These can be updated based on new knowledge and consolidated into the legislation.

Minimum required performance level (MRPL): This refers to a legal requirement for the

performance of the analytical method used for monitoring food of animal origin samples. The

requirement specifies an amount or concentration of analyte in the sample that has to be

reliably detected by the method. That is, the method LOD must be lower than the MRLP

value for the method to be fit for purpose.

NFSA: The Norwegian Food Safety Authority.

Parameter: A chemical, physical or microbiological property whose value describes or

characterises the sample. In this report the term is used for the concentrations of chemical

species of drugs, pollutants or additives or the assay results for physical objects or

microbiological or parasitic organisms in the sample.

Pesticide: A chemical substance used to kill, suppress or counteract pests, like insects, fungi,

weeds and diseases. Its primary use is for crop protection and disease control. Widespread use

has made some pesticides into environmental pollutants and potential food safety hazards.

PCB7, PCB6, sum of 6-PCBs or “indicator PCBs”: A selection of initially seven Poly

Chlorinated Biphenyls (PCBs) congeners that were recommended by the International

Council for the Exploration of the Sea (ICES) for use in the monitoring of pollution in the

marine environment. In EU legislation it was implemented as the shorter PCB6 list to avoid

overlap with the DLPCBs list. PCB-118, is one of the twelve dioxin-like PCBs.

POPs: Persistent Organic Pollutants. These are organic compounds with a negative impact on

the environment and/or on food safety due to toxic effects. POPs are persistent compounds

that will remain in the environments for a long time.

TE and SUM of TE: In the dioxin and dioxin like class of compounds the toxic equivalent

values (TE) measure the effective toxicity of the compound, expressed as a concentration. The

value is the product of the analytical concentration and a toxicity factor (WHO TEF 2005, see

the separate entry for TEF). The sums of TE values of related congeners like the furans, the


10

dioxins or the dioxin like PCBs, or the total sum of TE provides the combined toxicity of the

relevant congener groups.

TEF-1998 and TEF-2005: These are two lists of toxicity factors for dioxins, furans and

dioxin-like PCB congeners issued by the World Health Organisation WHO. These values are

called “Toxicity equivalent factors”, TEF. The first list was published in 1998 and the factors

were updated in a new list in 2005. The factors are relative toxicity data with no unit of

measurement. In 2012 the TEF-2005 list replaced the TEF-1998 list in the EU legislation.

Third country: Non-EU member state, or a state with no agreement with the EU on a

common border control.

Tissue: The samples received were whole fish, liver or muscle with skin and bone. From

crustaceans the samples were either whole body, white meat (muscle) or brown meat

(entrails). For cephalopods the received samples were whole body, mantle or muscle from the

tentacles.

TVB-N, Total volatile basic nitrogen: a chemical analysis used to assess spoilage in food.

TBARS: Thiobarbituric acid reactive substances: A chemical analysis used to assess

rancidity (per-oxidation of lipids) in food.

Upper bound sum (UB-sum), medium bound (MB) or lower bound (LB) sums: When a

concentration is found to be below the analytical method-s LOQ, its value is reported as:

“<LOQ” since the concentration cannot be assigned a reliable numerical value. If the

concentration is to be used as a part of a sum of concentrations, e.g. to calculate a mean value,

several strategies could be used: “Lower bound” sums: All values <LOQ are added to the sum

as 0.0. “Upper bound” sum (UB): All values <LOQ are added to the sum by their

corresponding LOQ value. “Medium bound” sum: all values <LOQ are added to the sum by

the corresponding value (0.5*LOQ). Previously the use of LB sums was the norm in food

safety evaluations, and this is still often used in environmental chemistry. While the MB sum

would provide the most realistic value, UB sums are now often preferred in food safety

evaluation. It provides a worst case scenario. In this report all mean- and sum-values are UB

based unless specified differently.

Commission regulation (EC) No 1881/2006 defines the maximum limits for dioxins, furans

and dioxin-like PCBs in terms of the value of their UB TE sums.

Wet weight and dry weight (w.w. and d.w.): The weight of the sample with natural

moisture present and the weight after drying. When concentrations units like μg/kg are used,

one should always specify whether d.w. or w.w. is used.


11

3. Introduction

3.1. Background and purpose

The European Economic Area (EEA) was established on 1 January 1994 following an

agreement between the member states of the European Free Trade Association (EFTA) and

the European Community, later the European Union (EU). As a member of the EEA, Norway

is a part of the EU external border control system. Since 1999, veterinary control based on

current EU legislation has been carried out in Norway, on food and feed products imported

from outside the EU/EEA area. The Norwegian Food Safety Authority (NFSA) is the

competent authority regarding veterinary border control.

Member States must have a monitoring plan with the objective to monitor conformity with

Community legislations, to detect residues, pathogenic organisms or other substances

dangerous to humans, animals or to the environment.

In cooperation with NFSA, NIFES have performed the analyses of the marine and seafood

samples in this monitoring programme and written this report.

This monitoring programme is part of the system that ensures that consignments of food from

third countries are rendered OK for free circulation between member countries as they are of

no danger to human (or animal) health.

The results of the laboratory tests from each Member State (including Norway) are reported to

the Commission monthly. The results are used for evaluating or planning the protective

measures in response to non-compliant foods and food stuffs from certain countries.

3.2 The legal foundation

The activity has been carried out in accordance with Commission Regulation (EC) No

136/2004, Annex II, Part 1.

3.3. The planning and scope of the work

The plans and procedures for this work target the most potent hazards associated with the

different kind of imports. The potential hazards were estimated from the compositional nature

of the different products, from the results from previous monitoring, on the geographical

origin of the samples, on the expected import frequency and on the information available in

the RASFF system. RASFF (Rapid Alert System for Food and Feed) is an EEA wide system

for exchange of information regarding non-compliant food and feed imports.

Due to the risk based nature of the monitoring, the data does not provide a statistically

representative picture of the consignments that cross our borders. But the chosen approach

enhanced the chance of finding non-conforming consignments. The data presentation is based

on maximum values and the number of non-conforming samples. Thus the report should be

http://en.wikipedia.org/wiki/European_Free_Trade_Association

http://en.wikipedia.org/wiki/European_Communities

http://en.wikipedia.org/wiki/European_Union


12

read as a worst case evaluation rather than as a representative picture of the imported sea

food.

4. Materials and methods

4.1. Sampling

The samples were taken from imported consignments from third countries that pass through

the official Norwegian BIPs. Seafood and marine products intended for direct human

consumption is the primary focus, but samples from marine raw materials intended for feed or

food production could also be sampled.

4.2. Sample reception, registration and pre-analytical sample handling

The samples from the BIPs are received in the NIFES sample reception unit. The sample is

documented by photography as it arrives in the sample reception unit and the relevant sample

identity, a lab-id number (journal number), and sample type and associated information are

documented in a Laboratory Information Management System (LIMS). LIMS handles user

privileges in such a way that identifying information is unknown to lab-staffs carrying out the

analytical work. Microbiological analyses are normally performed before other sample

handling to prevent potential microbial contamination on samples to interfere with the results

from that assay.

In the reception unit the sample is further prepared for analysis and then split in sub-samples

(aliquots) for the different assays and analyses. Each aliquot is stored properly to protect it

from contamination and storage effects that may interfere with the results from the assay it is

intended for.

For analysis of the edible part, unless otherwise stated, the muscle was selected. For species

with a given maximum value of undesirables, the tissue parts defined by the legislation were

always selected. In cephalopods the cuttlebone (gladius) was removed prior to analysis. For

products that was intended to be eaten whole, the whole was prepared for analysis

4.3. Chemical analytical methods and microbiological assays

The methods and the laboratory procedures used were accredited in accordance with the

standard ISO 17025, unless otherwise specified. A summary of the analytical methods used

for chemical parameters is listed in Table 15 in Annex 3. The table provides some method

performance data such as the LOQ values. Some parameters have been analysed by

subcontractors. When a subcontractor has been used this information is presented as well as a

summary of the analytical method performance data. Unless stated differently, the sample

preparation and analytical activity were carried out by the same procedures that were

presented in the report for this monitoring programme for the years 2006-2010. (Hove,


13

Lunestad, Holmelid and Måge, 2012. Report on Monitoring programme for veterinary control

on fisheries products imported to Norway from third countries - In accordance with

Commission Regulation (EC) No 136/2004, Annex II, Part 1. Results from the period 2005 to

2010). Section 4.3.1 in this report provides a summary of each new or modified method. The

analytical subcontractors are presented in section 4.3.2.

4.3.1 Quality assurance

For all methods, except for the dioxin method, a quality control sample (QCS) with a known

composition and concentration of target analyte, is included in each analytical series. A series

is equivalent to the analytical capacity for one day. The dioxin method quantification

principle is based on the isotope dilution method which integrates a higher level of quality

assurance in the method. Thus the frequency of the QCS analysis is reduced to allow a higher

analytical capacity for the dioxins method.

For all methods the QCS results are checked to be within pre-defined limits before the results

from a series are approved. With a certain frequency also a "blank analysis" routine is

performed in which a full analysis is carried out without a sample. If a positive value is found

for this “sample” this reflects a contamination of reagents or equipment that could affect the

results of the actual samples. All methods are regularly verified by participation in inter

laboratory proficiency tests, and by analysing certified reference material of relevant test

materials (CRM). The results for the verification should be within pre-defined limits before

the method is approved for continued use.

4.4 Other analytical methods

4.4.1. Method for oil authentication

Edible oils of marine origin are made from many different marine species. In this monitoring

programme, authentication of the species versus labelling of “marine oils” was carried out

through quantitative analysis of the composition of fatty acids and phytosterol compounds in

the oil. The fatty acid profile varies between different marine species and differs from the

composition in plant oils. Thus the fatty acid profile is informative for oil authentication.

Phytosterol compounds are found in terrestrial plants, but not in significant quantities in

marine oils. Colour, scent and appearance are also relevant for oil authentication purposes.


14

4.4.2. Analytical sub-contractor

Eurofins carried out the quantitative analysis for nitrofuranes and PAH. The analytical

principles involved were described in the report for this monitoring programme for the years

2006-2010 (Hove, Lunestad, Holmelid and Måge, 2012. Report on Monitoring programme for

veterinary control on fisheries products imported to Norway from third countries - In

accordance with Commission Regulation (EC) No 136/2004, Annex II, Part 1. Results from

the period 2005 to 2010).

4.5 Application of maximum limits to non-standard products

Most maximum limits are defined for certain tissues like fish muscle, or for the meat of

crustaceans. For products that fit the description in the legislation the application of the

legislation to the analytical result is straight forward, taking into account the analytical

uncertainty. For products intended to be eaten whole, the whole product was analysed and the

maximum limit applied to the result. For samples that were imported in a pre dried state,

processed or otherwise treated in a way that renders the maximum limit not directly

applicable, the procedure in regulation 1881/2006 article 2 was applied. This mean that for the

evaluation of legal conformity an “adjusted” maximum limit is calculated in accordance with

the effects of dilution, drying and other processing to find a maximum value applicable to that

sample. For predried samples, the actual original moisture contents were generally unknown.

NIFES then applied an estimated original moisture content based on our experience with

similar products in order to carry out the legal conformity evaluation.


15

5. Results and discussion

A total of 144 samples, all sampled at the BIPs, were analysed in this monitoring programme.

Most of the samples were examined by a range of analytical parameters. The sampling at the

BIPs, as well as the selection for each sample of the relevant chemical and microbiological

analytical parameters, was carried out according to a plan, as described in section 4.2.

5.1. Microbiology

The results from the microbiological examinations are listed in Table 1. A total of 140

samples were tested for microorganisms in a range of assays.

A total of 59 samples (65 %) had general plate counts at 20°C above the value of 1000 cfu/g.

The highest counts were 1.3 x 106 in one sample of cod from China and 1.2 x 106 bacteria in

one sample of swordfish imported from Sri Lanka.

The aerobic plate counts on non-selective agar growth medium, incubated at 30°C, were

generally low: 18 samples (37 %) had plate counts above the value of 1000 cfu/g. The highest

number was 3.4 x 106 bacteria/g, found in a processed product imported from Vietnam.

The number of H2S producing bacteria at 20°C incubation was generally low in all samples.

Ten of the 91 examined samples (11 %) had H2S producing bacteria in concentrations of 1000

bacteria/g or higher. The highest number was found in the same sample of swordfish from Sri

Lanka, with 1.7 x 105 bacteria/g.

One processed product and six samples of bivalves were examined for E. coli by the Donovan

MPN method. All seven samples gave counts <20 bacteria/100 gram sample material, and

were thus compliant with EU regulations. The results for determination of coliforms and E.

coli in 61 samples by the agar plate assay were all under the limit of detection, which is 10

bacteria/g, for E. coli. However, 2.0 x 103 and 1.4 x 103 coliforms/g, respectively, were found

in one sample of scampi from Vietnam and in one sample of swordfish from Sri Lanka.

The examination for faecal indicator organisms by the MPN method also generally showed a

low prevalence of coliforms, thermotolerant coliforms and faecal coliforms. Of the 39

samples examined by the MPN method, only one of the coliform assays was above the level

of three bacteria/g: four bacteria/g sample material was found in a sample of trout from

Thailand

The number of Staphylococcus aureus, sulphite reducing clostrides and bacteria in the family

Enterobacteriacae, were generally under their respective levels of detection. Two samples

gave counts of 1.1 x 105 and 1.5 x 105 sulphite-reducing bacteria/g, respectively, for a

processed product from Vietnam and a sample of prawns from Canada.


16

For enterococci, two of 101 examined samples were above the detection limit of 100 cfu/g.

The numbers of bacteria were 400 /g in both samples, which were of scampi imported from

Vietnam.

In 2012, 93 samples were analysed for L. monocytogenes. The presence of this pathogen was

detected in one sample of trout from Peru and one sample of salmon from Chile. Both

samples contained <100 bacteria/g.

Salmonella was detected in one sample of raw, frozen scampi imported from Vietnam. The

serovar of the isolate was found to be S. Weltevreden. Other consignments from the same

producer in Vietnam were found by Eurofins to harbour S. Newport and S. Kentucky. The

consignments consisting of 18 metric tonnes distributed throughout Norway were withdrawn

from the market.

Vibrio alginolyticus was detected in one sample of pollock fillet imported from Russia. This

Vibrio species is not generally classified as a food borne pathogenic species.

5.2. Parasites

A total of 60 samples of fish were subjected to a parasitological assay. The data is listed in

Table 2. Nematodes were found in 17 samples (28%). The highest numbers of nematodes

were found in a sample of Greenland halibut (32 nematodes). Nematodes were also found,

with a lower density of infection, in samples of cod, haddock, redfish, saithe and mackerel.

5.3. Drug residues and dyes

Eighteen samples of farmed fish, shellfish, crustaceans or mixed seafood products were

examined for residues of illegal drugs and dyes. The leuco forms of crystal violet and

malachite green are generated as biodegradation products in fish treated by the parent

compounds. A presence of any of the leuco-compounds would be as indicative of illegal use

as the presence of the parent compounds. The data are listed in Table 3.

The samples were analysed for the presence of chloramphenicol and for the nitrofurane

metabolites 3-amino-2-oxazolidinone (AOZ), 3-amino-5-morpholinomethyl-2-oxazolidinone

(AMOZ), 1-amino-hydantoin (AHD) and semi-carbazide (SEM). The data are listed in Table

4. No residue of drugs or dyes could be detected in any of the samples.

5.4. Chemical spoilage and rancidity indicators

A total of 18 samples (different from those above), all from marine fish, were analysed for

chemical spoilage parameters. The data listed in Table 5 include histamine, the TBARS

rancidity data and the total volatile basic nitrogen data (TVB-N). One sample of tuna from Sri

Lanka and one from Vietnam had levels of histamine of 32 and 33 mg/kg w.w respectively.

Three samples had values for TBARS above10 nmol/g: One sample of mackerel re-imported

from Turkey (60 mol/g w.w), one sample of tuna from Vietnam (35 mol/g) and one sample of


17

“fish snacks” from Thailand (11nmol/g w.w.). The highest values of TVB-N was found in a

tinned tuna sample from Thailand (35.4 mg/100g w.w), and in a sample of tuna from Sri

Lanka (20.5 mg/100g w.w.). The cited values are in themselves not indicative of a hazard to

human health. They do however indicate that the mentioned samples have been exposed to

improper storage or transport conditions.

5.5. Oil authentication

One oil samples was assayed for biological species authentication. It was labelled “cuttlefish

oil”. The data for fatty acid composition are listed in Table 6, and the data for sterol

composition are listed- in Table 7. From the data, we may conclude that the labelled

biological species was probably correct.

5.6. Heavy metals

A total of 109 samples were analysed for the elements arsenic, cadmium, lead and mercury.

The data are listed in Table 8. The maximum levels are summarised in Annex 2, Table 14.

5.6.1. Arsenic (As)

There is no legal limit for arsenic in fish and fishery products. In marine species, arsenic is

mainly present in chemical species of low toxicity, such as arsenobetaine. This differs from

food of terrestrial origin where inorganic toxic arsenic species give a significant contribution

to the total arsenic concentration. The highest concentration of total arsenic in our samples

was 27 mg/kg found in a cod imported from Russia. From the data found in the NIFES sea

food database this value lies in the normal range. Given the low toxicity of arsenic in lean fish

fillets, this value gives no reason for concern. (NIFES Sea food database:

http://www.nifes.no/index.php?page_id=137&lang_id=2).

5.6.2. Cadmium (Cd)

The highest elemental concentration of cadmium was 1.7 mg/kg w.w., in a sample of squid oil

imported from South Korea. There is no maximum limit for cadmium in oil. A sample of

lobster from Canada was measured to 0.51 mg/kg w.w. while the maximum level for lobster

is 0.5 mg/kg w.w. Due to the analytical measurement uncertainty the sample was still

considered to be in compliance with legislation.

5.6.3. Mercury (Hg)

No values of elemental mercury were found above their respective maximum levels. Tuna and

swordfish have a permitted maximum level of 1.0 mg Hg/kg w.w. One sample of tuna and

one sample of swordfish were above the maximum level of 0.5 mg Hg/kg w.w. used for most

other fish species.

http://www.nifes.no/index.php?page_id=137&lang_id=2


18

5.6.4. Lead (Pb)

No value of elemental lead was found above the maximum level. And the measured levels are

low. One sample of prawns imported from Thailand still stands out with a high level with a

value of 0.44 mg/kg w.w. but this is well below upper levels for this food.

5.7. Persistent organic pollutants (POPS)

Samples were analysed for dioxins, furans, dioxin-like PCBs, non dioxin-like PCBs (PCB6)

brominated flame retardants, chlorinated pesticides and PAH. Since the POPs are lipophilic

compounds, they are found in the highest levels in fatty tissues. In what we regard as lean

fish, they are found mainly in the liver.

5.7.1. The dioxins; PCDDs, PCDFs and DLPCBs

A total of 31 samples were analysed. The data are listed in Table 9. All analytical levels are

presented as TE values (toxic equivalent value, see chapter 3 for the definition). Regulatory

limits for these compounds are established for several food products (Annex 2, Table 14). All

data and all regulatory limits in seafood are on a w.w. basis.

One sample of squid oil exceeded the limit for the sum of total TE with a sum of 41 pg/g TE.

The DLPCBs were the compounds responsible for the high value. The squid sample was of

Todarodes sagittatus, the European flying squid (cuttlefish). This finding is in line with

results from previous years showing that samples of this species may have high values. Also,

the second highest sample, sample 2012-1454/1, a crude oil from the USA was measured to

contain 5.0 pg/g TE w.w. This is equal to the maximum a value and the sample will be

discussed further later on.

5.7.2. The indicator PCBs

The data for these PCBs are listed in Table 10. The analytical value of PCB-118 is also given

for compatibility with the reports from previous years. PCB-118 is not part of the sum 6-

PCBs, but was part of the previously used sum 7-PCBs. A total of 4 samples were analysed.

No sample exceeded its maximum limit.

5.7.3. Polybrominated diphenyl ethers (PBDE)

The data are listed in Table 11. A total of 29 samples were analysed. No maximum levels are

established. The two highest analytical values for the sum 7-PBDE were 33 and 14 µg/kg

w.w., respectively, found in two samples of marine oil, one from the USA and one from South

Korea. The PBDE-47 congener was the main contributor to the sum of 7 PBDEs. The oil from

South Korea also had high values of Cd and it exceeded the limit for dioxins. The oil from

USA had also a noticeable level of dioxins, but the sample was not measured for Cd.

5.7.4. Pesticides

The data on pesticides analyses are listed in Table 12 and the origin og the samples are given

in Table 1. Only halogenated pesticides were included in the monitoring. There are no legal


19

limits for these compounds in fish and fishery products except when they are used in feeds. A

total of 22 samples were analysed. Most of the measured compounds were not detected or

were measured in very low levels. The levels measured in sea food were generally lower than

the values found in oil. Like in previous years DDT and its closely related compounds were

found in the highest levels. The DDTs had their maximum values in the South Korean squid

oil with a level of 100 µg/kg w.w for p,p’-DDT. This was the highest concentration measured

of all the undesirables. DDE followed by p,p’-DDD with 74 and o,p’- DDD with 19 µg/kg

w.w. in the same oil. The American oil had almost as high values. The highest level of

dieldrin was 29 μg/kg w.w. in the American oil, followed by Hexachlorobenzene and trans-

nonachlor with highest values of 22 and 20 μg/kg w.w. respectively, in the South Korean oil.

5.7.5. Polyaromatic hydrocarbons, PAH

PAH is a whole class of compounds with many individual compounds suspected of some

level of carcinogenic activity. A new set of maximum levels for the LB-sum of four PAHs

(PAH4) were set into force from September 20121. (See chapter 3 for the definition of LB-

sum). The separate maximum level for benzo(a)pyrene (BaP) is maintained for most foods.

But the previous maximum limit for “muscle meat of fish other than smoked fish” was

removed. The four compounds in the PAH4 sum are: BaP, Benzo(a)anthracene,

Benzo(b)fluoranthene and chrysene. A summary of the limits are provided in Table 14 in

Annex 2.

The data are listed in Tables 13. The values for BaP are highlighted in the table. No sample

exceeded the limit for BaP. One of the 23 analysed samples exceeded the maximum level for

the PAH4. It is the same South Korean squid oil sample that had high levels of cadmium,

dioxins and PBDEs. The sample was taken prior to the date of the implementation of the new

legislation. The American oil had low levels of PAH.

1 Commission Regulation (EU) 835/2011 of 19 August 2011.

ANNEX 1: DATA TABLES

Table 1. Microbiological parameters, n=140, na: data not available

Aerobic plate count (cfu/g), agar method

Indicator organisms

(cfu/g) by agar method

Faecal indicator organisms (cfu/g) by agar method

Faecal indicator organisms by MPN method

Specific pathogens

30°C

20°C

En

tero

co

ccu

s

Sta

ph

ylo

co

cc

us

au

reu

s

Su

lph

.-red

. bac

t.

En

tero

bac

teria

ce

ae

Co

liform

ba

cte

ria

E. c

oli

Th

erm

oto

lera

nt c

olifo

rms

E. c

oli

E. c

oli

Co

liform

ba

cte

ria

Th

erm

oto

lera

nt c

olifo

rms

Lis

teria

mo

no

cyto

gen

es

Salm

on

ella

sp

.

Vib

rio

H2S prod.

PC Donovan Qual. Quant.

Journal nr. From Species Tissue Incub.

test /g /g /g /g /g /g /g /g /g /g /100 g /g /g /g /25 g CFU/g /25 g /20 g

2012-96/1 Russia Redfish Fillet

<1000 2000 <100

<3 <3 <3 neg.

neg. neg.

2012-102/1 Thailand Tuna n.a. neg. <1000

2012-110/1 India Red snapper n.a.

11000 560000 <100

<3 <3 <3 neg.

neg. neg.

2012-193/1 Russia Cod Fillet

<1000 320000 <100

<3 <3 <3 neg.

neg. neg.

2012-194/1 Russia Cod Roe

<1000 4000 <100

<100

<3 <3 <3 neg.

neg.


<1000 2000 <100

<100

<3 <3 <3 neg.

neg.


<1000 57000 <100

<100

<3 <3 <3 neg.

neg.


<1000 11000 <100

<100

<3 <3 <3 neg.

neg.

2012-262/1 Russia Greenland

halibut Fillet

<1000 25000 <100

<3 <3 <3 neg.

neg. neg.

2012-342/1 Canada Lobster Whole

<1000 <1000 <100

<3 <3 <3 neg.

neg. neg.

2012-405/1 Thailand Trout Fillet

<1000 5000 <100

<3 4 <3 neg. <100 neg. neg.

2012-406/1 Thailand Salmon Fillet

<1000 1000 <100

<3 <3 <3 neg. <100 neg. neg.

2012-464/1 Russia Redfish Decapitated

4000 310000 <100

<3 <3 <3 neg.

neg. neg.


<1000 6000 <100

<100

<3 <3 <3 neg.

neg.

2012-466/1 Sri Lanka Sword fish n.a.

6000 54000 100

<3 <3 <3 neg.

neg. neg.

2012-467/1 Japan Tuna n.a.

<1000 <1000 <100

<3 <3 <3 neg.

neg. neg.

2012-473/1 Greenland Cod Fillet

<1000 25000 <100

<3 <3 <3 neg.

neg. neg.

2012-474/1 Philippines Processed

product Sardines neg. <1000

2012-476/1 Vietnam Scampi Peeled

<1000 3000 <100

<3 <3 <3 neg.

neg. neg.

2012-490/1 Chile Oil Processed

<1000

<100

<10 <10

neg.

2012-491/1 Peru Oil Processed

<1000

<100

<10 <10

neg.

2012-521/1 China Cod Fillet

<1000 <1000 <100

<3 <3 <3 neg.

neg. neg.


<1000

<100 <100 <100

<10 <10

neg.


21

2012-532/1 USA Oil Alaska pollock

<1000

<100

<10 <10

neg.


<1000 43000 <100

<3 <3 <3 neg.

neg. neg.


63000

<100 <100 <100

<10 <10

neg.

2012-536/1 China Redfish Fillet

141000

<100 <100 <100

<10 <10

neg.

2012-537/1 China Clipfish Fillet

<1000

<100 <100 <100

<10 <10

neg.

2012-538/1 Thailand Prawns Freeze-dried

5000

<10

<10 <10

neg.

2012-539/1 Peru Oil Crude fish oil

<1000

<100

<10 <10

neg.

2012-540/1 Chile Oil Semi-refined

<1000

<100

<10 <10

neg.

2012-541/1 Vietnam Oil Tuna oil

<1000

<100

<10 <10

neg.

2012-542/1 South Korea Oysters Muscle

<1000 1000 <100

<20

neg. <100 neg. neg.


halibut Fillet

<1000 10000 <100

<3 <3 <3 neg.

neg. neg.

2012-564/1 Russia Pollock Fillet

<1000 147000 <100

<3 <3 <3 neg.

neg. neg.

2012-565/1 Russia Wolffish Fillet

<1000 <1000 <100

<3 <3 <3 neg.

neg. neg.

2012-566/1 Russia Halibut Fillet

<1000 <1000 <100

<3 <3 <3 neg.

neg. neg.


<1000 72000 <100

<3 <3 <3 neg.

neg. neg.

2012-568/1 Russia Redfish Fillet

<1000 280000 <100

<3 <3 <3 neg.

neg. neg.


<1000 64000 <100

<3 <3 <3 neg.

neg. pos.

2012-577/1 Russia Haddock Fillet

<1000 34000 <100

<3 <3 <3 neg.

neg. neg.

2012-619/1 Morocco Oil Marine fish oil

<1000

<100

<10 <10

neg.

2012-627/1 Thailand Cod Fillet

17000

<100

<10 <10

neg.

neg.

2012-628/1 Thailand Cod Fillet

46000

<100 <100 <100

<10 <10

neg.

2012-666/1 USA Red king

crab Claw

<1000

<100 <100

<10 <10

neg. neg.


<1000 18000 <100

<3 <3 <3 neg. <100 neg. neg.


10000 870000 <100

<3 <3 <3 neg. <100 neg. neg.


<1000 151000 <100

<3 <3 <3 neg. <100 neg. neg.


<1000 200000 <100

<3 <3 <3 neg.

neg. neg.


<1000 10000 <100

<3 <3 <3 neg.

neg. neg.


halibut Fillet

<1000 125000 <100

<3 <3 <3 neg.

neg. neg.


<1000 71000 <100

<3 <3 <3 neg.

neg. neg.


<1000 46000 <100

<3 <3 <3 neg. <100 neg. neg.


<1000 80000 <100

<3 <3 <3 neg. <100 neg. neg.


<1000 18000 <100

<3 <3 <3 neg. <100 neg. neg.


<1000 229000 <100

<3 <3 <3 neg.

neg. neg.

2012-731/1 Canada Lobster Raw, frozen

<1000 91000 <100

<3 <3 <3 neg.

neg. neg.


<1000 <1000 <100

<100

<10

neg.

neg.

2012-1181/1 Sri Lanka Tuna Muscle

<1000 <1000 <100

<10

neg.

neg. neg.

2012-1182/1 Sri Lanka Parrotfish Whole

<1000 <1000 <100

<10

neg.

neg. neg.


<1000 <1000 <100

<10

neg.

neg. neg.

2012-1295/1 Japan Yellowtail Fillet

<1000 <1000 <100

<10

<10

neg. <100 neg. neg.

2012-1408/1 Russia Redfish Decapitated

<1000 11000 <100

<10

<10

neg. <100 neg. neg.

2012-1411/1 Morocco Sardines Oil

<1000

<100

<10

neg.


22


<1000 <1000 <100

<10

<10

neg. <100 neg. neg.

2012-1420/1 China Monkfish Fillet

<1000 10000 <100

<10

<10

neg. <100 neg. neg.

2012-1421/1 South Korea Squid Oil

<1000

<100

<10

neg.

2012-1422/1 Thailand Tuna Oil

<1000

<100

<10

neg. neg.

2012-1423/1 South Africa Hake Fillet

<1000 56000 <100

<10

<10

neg. <100 neg. neg.

2012-1424/1 Canada Prawns Peeled

6000

<100 <100

<10

neg. neg.


<1000 1340000 <100

<10

<10

neg. <100 neg. neg.

2012-1426/1 USA Lobster Processed

<1000

<100 <100

<10

neg.

2012-1454/1 USA Gulf

menhaden Oil

<1000

<100

<10

neg. neg.

2012-1619/1 USA Scallop Muscle

<1000 2000 <100

<20

neg. <100 neg. neg.


<1000 10000 <100

<20

neg. <100 neg. neg.

2012-1621/1 Vietnam Scampi Whole

1000 68000 <100

2000

<10

neg. <100 neg.

2012-1622/1 Thailand Fish snack n.a.

<1000

<100 <100 <100

<10

neg. <100 neg. neg.

2012-1623/1 Thailand Eel Muscle

<1000 <1000

<10

<10

neg. neg.

2012-1624/1 Canada Surf clam Raw, frozen

<1000 <1000 <100

<10

<10

neg. <100 neg. neg.

2012-1625/1 Thailand Processed

product Mixed

product <1000 3000 <100

<10

<10 <20

neg. <100 neg. neg.

2012-1627/1 Taiwan Processed

product Mixed

product <1000 <1000 <100

<10

<10

neg. <100 neg. neg.

2012-1634/1 Vietnam Scampi Raw, frozen

1000 108000 400

<10

<10

neg.

pos. neg.


<1000 <1000 <100

<20

neg. <100 neg. neg.

2012-1636/1 Vietnam Octopus Tentacles

<1000 1000 <100

<10

<10

neg. <100 neg. neg.

2012-1638/1 Vietnam Scampi Raw, pealed

<1000 14000 <100

<10

<10

neg. <100 neg. neg.

2012-1639/1 Vietnam Pangasius n.a.

<1000 18000 <100

<10

<10

neg.

neg. neg.

2012-1648/1 Philippines Milkfish n.a.

<1000 1000 <100

<10

<10

neg.

neg. neg.

2012-1649/1 Peru Trout n.a.

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1650/1 Peru Trout n.a.

<1000 152000 <100

<10

<10

pos. <100 neg. neg.

2012-1652/1 Canada Lobster Whole, cooked

<1000

<100 <100

<10

neg. neg.

2012-1653/1 Canada Lobster Cooked

<1000

<100 <100

<10

neg. neg.

2012-1655/1 Vietnam Crab Claw meat,

cooked 1000

<100 <100

<10

neg.

2012-1657/1 Morocco Sardines Sardines in

oil neg. <1000


product Shrimp paste

128000

<100

<10

neg. neg.

2012-1767/1 Thailand Scampi Spring rolls

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1769/1 Thailand Halibut Processed

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1770/1 China Squid Processed

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1771/1 Vietnam Pangasius n.a.

<1000 1000 <100

<10

<10

neg.

neg. neg.

2012-1772/1 Vietnam Barramundi Fillet

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1773/1 Taiwan Octopus Dried

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1774/1 Canada Scallop Wild caught

<1000 10000 <100

<20

neg.

neg.

2012-1775/1 Vietnam Processed

product Dried fish

3400000

<100 <100 10700

1230

neg. neg.


23

2012-1792/1 Canada Prawns Hel

34000

<100 300

<10

neg. neg.


11000

<100 14500

<10

neg. neg.


5000

<100 100

<10

neg. neg.

2012-1795/1 Chile Salmon Fillet

<1000 7000 <100

<10

<10

pos. <100 neg. neg.

2012-1797/1 Sri Lanka Sword fish Fillet

166000 1240000 <100

1440

<10

neg.

neg. neg.

2012-1807/1 Vietnam Scampi n.a.

<1000 9000 <100

<10

<10

neg.

neg. neg.

2012-1808/1 Canada Prawns Cooked, peeled

5000

<100 <100

<10

neg. neg.


<1000 55000 <100

<10

<10

neg.

neg. neg.

2012-1811/1 Canada Prawns Cooked, peeled

8000

<100 <100

<10

neg. neg.

2012-1812/1 Canada Lobster Bodies

<1000 9000 <100

<10

<10

neg.

neg.

2012-1813/1 Thailand Wolffish Processed

product neg. <1000

<100 <100 <100

<10

neg.

2012-1816/1 China Tilapia Whole, frozen

<1000 1000 <100

<10

<10

neg.

neg.

2012-1817/1 Thailand Crab Crab flakes

<1000

<100

<10

neg. neg.

2012-1818/1 Turkey/Norway Mackerel Fillet

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1819/1 Sri Lanka Tuna Fillet

<1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1820/1 Vietnam Tuna Fillet

<1000 3000 <100

<10

<10

neg.

neg. neg.

2012-1823/1 Japan Yellowtail Whole round,

chilled <1000 <1000 <100

<10

<10

neg.

neg. neg.

2012-1824/1 Canada Lobster Live lobster

9000 229000 <100

<10

<10

neg.

neg. neg.

2012-1871/1 Canada Lobster Live lobster

<1000 10000 <100

<10

<10

neg.

neg. neg.

2012-1872/1 Peru Crab Cooked crab

meat <1000

<100 <100

<10

neg.

2012-1880/1 Vietnam Processed

product Spring rolls

10000

<100 <100 <100

<10

neg.

neg. neg.

2012-1881/1 Canada Lobster Raw, frozen

<1000 <1000 <100

<10

<10

neg.

neg.

2012-1882/1 Thailand Shortfin lizardfish

Fish snack

<1000

<10

<10

neg.


430000

<100 <100 <100

<10

neg. neg.

2012-1884/1 China Pollock Fillet

<1000 24000 <100

<10

<10

neg.

neg. neg.

2012-1885/1 Vietnam Scampi Processed

product 6000 90000 400

<10

<10

neg.

neg. neg.

2012-1890/1 Canada Prawns Whole

4000

<100 <100

<10

neg. neg.

2012-1905/1 Vietnam Scampi Raw

<1000 26000 <100

<10

<10

neg.

neg.

2012-1917/1 Canada Various fish Cat fee, dried

25000

<100

<10

neg. neg.

2012-1918/1 Canada Scallop Muscle

1000 66000 <100

<20

neg.

neg.

2012-1919/1 Thailand Gouramy/ Mudfish

Pickled fish neg. <1000

2012-1920/1 Thailand Crab Claw, tinned neg. <1000

2012-1921/1 Norway/Vietnam Cod Fish meal

<1000

<10

<10

neg.


product Shrimp paste

45000

<100

<10

neg.

2012-1951/1 Norway/USA Marine fish Oil

<1000

<100

<10

neg. neg.


24


<1000 <1000 <100

<10

<10

neg.

neg.


<1000

<100 <100 <100

<10

neg. neg.

2012-1954/1 China Pollock Fillet

<1000 25000 <100

<10

<10

neg.

neg.


25

Table 2. Number of nematodes, n=60, n.a. = data not available

Journal Nr. Imported from Group Species Tissue Preservation # Nematodes

2012-96/1 Russia Marine fish Redfish Muscle Frozen 16

2012-110/1 India Marine fish Red snapper Muscle Frozen 0

2012-193/1 Russia Marine fish Cod Muscle Frozen 0

2012-262/1 Russia Marine fish Greenland halibut Muscle Frozen 15

2012-405/1 Thailand Marine fish Trout Muscle Frozen 0

2012-406/1 Thailand Marine fish Salmon Muscle Frozen 0


2012-466/1 Sri Lanka Marine fish Marlin Muscle Frozen 0

2012-467/1 Japan Marine fish Tuna Muscle Frozen 0

2012-473/1 Greenland Marine fish Cod Muscle Frozen 0

2012-521/1 China Marine fish Cod Muscle Frozen 4



2012-564/1 Russia Marine fish Saith Muscle Frozen 9

2012-565/1 Russia Marine fish Wolffish Muscle Frozen 0

2012-566/1 Russia Marine fish Halibut Muscle Frozen 0



2012-569/1 Russia Marine fish Saithe Muscle Frozen 3

2012-577/1 Russia Marine fish Haddock Muscle Frozen 1

2012-627/1 Thailand Marine fish Cod Muscle Frozen 0


26













2012-1181/1 Sri Lanka Marine fish Tuna Muscle Frozen 0

2012-1182/1 Sri Lanka Marine fish Parrot fish Muscle Frozen 0


2012-1295/1 Japan Marine fish Yellowtail Muscle Frozen 0



2012-1420/1 China Marine fish Wolffish Muscle Frozen 0

2012-1423/1 South Africa Marine fish Hake Muscle Frozen 0


2012-1623/1 Thailand Marine fish Eel Muscle Frozen 0

2012-1639/1 Vietnam Freshwater fish Pangasius Muscle Frozen 0

2012-1648/1 Philippines Marine fish Milkfish Muscle Frozen 0

2012-1649/1 Peru Marine fish Trout Muscle Frozen 0

2012-1650/1 Peru Marine fish Trout Muscle Frozen 0

2012-1769/1 Thailand Marine fish Halibut Muscle Frozen 1


27



2012-1771/1 Vietnam Freshwater fish Pangasius Muscle Frozen 0

2012-1772/1 Vietnam Marine fish Barramundi Muscle Frozen 0

2012-1795/1 Chile Marine fish Salmon Muscle Frozen 0

2012-1797/1 Sri Lanka Marine fish Marlin Muscle Frozen 0


2012-1816/1 China Marine fish Tilapia Muscle Frozen 0

2012-1818/1 Turkey Marine fish Mackerel Muscle Frozen 1

2012-1819/1 Sri Lanka Marine fish Tuna Muscle Frozen 0

2012-1820/1 Vietnam Marine fish Tuna Muscle Frozen 0

2012-1823/1 Japan Marine fish Yellowtail Muscle Frozen 0

2012-1884/1 China Marine fish Saithe Muscle Frozen 0


2012-1954/1 China Marine fish Saithe Muscle Frozen 0

Number of samples 60

Maximum number of

nematodes 32

Number of infected

fish 17


28

Table 3. Residues of veterinary medicine and prohibited compounds: Dyes, n=16. CV: crystal violet, LCV: leuco crystal violet, MG: malachite green LMG: leuco malachite green, BG: brilliant green

n.a. = not available, n.d.=not detected CV LCV MG LMG

BG

Journal Nr. Imported from Group Species Preservation LOD

0.3 µg/kg LOD

0.15 µg/kg LOD

0.15 µg/kg LOD

0.15 µg/kg LOD

0.15 µg/kg

2012-476 Vietnam Crustacean Scampi Frozen raw n.d. n.d. n.d. n.d

n.d

2012-542 S. Korea Farmed shellfish Oyster Frozen raw n.d. n.d. n.d. n.d

n.d

2012-1181 Sri Lanka Farmed fish Tuna Frozen raw n.d. n.d. n.d. n.d

n.d

2012-1295 Japan Farmed fish Yellowtail (Seriola sp.) Frozen raw n.d. n.d. n.d. n.d.

n.d.

2012-1625 Thailand Mixed Scampi, blue mussel, squid Frozen raw n.d. n.d. n.d. n.d

n.d

2012-1634 Vietnam Crustacean Scampi Frozen raw n.d. n.d. n.d. n.d.

n.d.

2012-1639 Vietnam Farmed fish Pangasius Frozen raw Muscles n.d. n.d. n.d. n.d

n.d

2012-1648 Philippines Farmed fish Milkfish Frozen raw n.d. n.d. n.d. n.d

n.d

2012-1650 Peru Farmed fish Trout Frozen raw n.d. n.d. n.d. n.d.

n.d.

2012-1767 Thailand Crustacean, spring rolls

Scampi Frozen raw n.d. n.d. n.d. n.d

n.d

2012-1771 Vietnam Farmed fish Pangasius Frozen raw Muscles n.d. n.d. n.d. n.d.

n.d.

2012-1772 Vietnam Farmed fish Barramundi Frozen raw n.d. n.d. n.d. n.d

n.d

2012-1795 Chile Farmed fish Salmon Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1807 Vietnam Crustacean Scampi Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1823 Japan Farmed fish Yellowtail (Seriola sp.) Frozen raw n.d. n.d. n.d. n.d. n.d.



29

Table 4. Residues of veterinary medicine and prohibited compounds: Chloramphenicol, nitrofuranes and their metabolites, n=18. AOZ: 3-amino-2-oxazolidinone, AMOZ: 3-amino-5-morpholinomethyl-2-oxazolidinone, AHD: 1-amino-hydantoin, SEM:

semicarbazide

n.a. = not available, n.d.=not detected Chlorampheni

col AHD AMOZ AOZ SEM

Journal Nr. Imported

from Group Species Preservation LOD

0.25 µg/kg LOD

1.0 µg/kg LOD

0.5 µg/kg LOD

0.5 µg/kg LOD

1.0 µg/kg


2012-542 S. Korea Farmed shellfish Oyster Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1181 Sri Lanka Farmed fish Tuna Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1295 Japan Farmed fish Yellowtail (Seriola sp.) Frozen raw n.d. n.d. n.d. n.d. n.d.


2012-1625 Thailand Mixed

Scampi, blue mussel,

squid Frozen raw n.d. n.d. n.d. n.d. n.d.


2012-1639 Vietnam Farmed fish Pangasius Frozen raw

Muscles n.d. n.d. n.d. n.d. n.d.

2012-1648 Philippines Farmed fish Milkfish Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1649 Peru Farmed fish Trout Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1650 Peru Farmed fish Trout Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1767 Thailand Crustacean, spring rolls

Scampi Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1771 Vietnam Farmed fish Pangasius Frozen raw

Muscles n.d. n.d. n.d. n.d. n.d.

2012-1772 Vietnam Farmed fish Barramundi Frozen raw n.d. n.d. n.d. n.d. n.d.

2012-1795 Chile Farmed fish Salmon Frozen raw n.d. n.d. n.d. n.d. n.d.


2012-1823 Japan Farmed fish Yellowtail (Seriola sp.) Frozen raw n.d n.d. n.d. n.d. n.d

2012-1905 Vietnam Crustacean Scampi Frozen raw n.d. n.d. n.d. n.d. n.d


30

Table 5. Levels of chemical spoilage and rancidity indicators, n=18.


from Group Species Tissue Preservation

Histamine mg/kg w.w.

TBARS nmol/g

w.w.

TVB-N mg/100g w.w.

2012-102/1 Thailand Marine fish Tuna Filet Tinned, in water <5.0 4.3 35.4

2012-193/1 Russia Marine fish Cod and haddock Filet n.a. n.a. n.a. 10.1

2012-405/1 Thailand Marine fish Trout Filet n.a. <5.0 <4.0 14.5

2012-406/1 Thailand Marine fish A. salmon Filet n.a. <5.0 5.3 12.3

2012-474/1 Philippine Marine fish Sardines Sardines in oil Tinned, in oil <5.0 n.a. n.a.

2012-537/1 Kina Marine fish Cod Whole gutted Dried n.a. n.a. 13.5

2012-627/1 Thailand Marine fish Cod Loins Smoked n.a. <4.0 8.7

2012-628/1 Thailand Marine fish Cod Loins Smoked n.a. <4.0 8.6

2012-723/1 Russia Marine fish Greenland halibut Filet n.a. n.a. <4.0 9.1

2012-1181/1 Sri Lanka Marine fish Tuna Muscle n.a. <5.0 <4.0 17.4

2012-1622/1 Thailand Marine fish Fish snacks Several snacks n.a. 11 n.a.

2012-1623/1 Thailand Marine fish Eel fillet Fresh n.a. n.a. 14.5

2012-1657/1 Morocco Marine fish Sardines Sardines in oil Tinned, in oil 9.1 13 8.6

2012-1795/1 Chile Marine fish A. salmon Filet n.a. n.a. n.a. 15.3

2012-1818/1 Turkey /Norway Marine fish Mackerel Filet n.a. <5 60 11.9

2012-1819/1 Sri Lanka Marine fish Tuna Filet Fresh 32 4.2 13.7

2012-1820/1 Vietnam Marine fish Tuna Filet Fresh 33 35 20.5

2012-541/1 Vietnam Marine fish Tuna Oil - <5.0 n.a. n.a.

Samples analysed 10 12 15

Maximum value 33 60 35.4


31

Table 6. Fatty acid composition for oil biological species authentication, mg/g (w.w.) and relative amounts (%), n=1.

Name

2012-1421 Squid oil

(see also appendix-3)

NIFES

accumulated

profile for squid

oil

Fatty acid mg/g % %

06:0 <0.01 <0.1 <0.1

08:0 0.16 <0.1 <0.1

10:0 0.31 <0.1 <0.1

12:0 0.17 <0.1 <0.1

14:0 27.03 3 3.9

14:1n-9 0.42 <0.1 0.1

15:0 3.91 0.4 0.4

16:0 134.8 14.8 13.1

16:1n-7 26.31 2.9 3

16:1n-9 3.1 0.3 0.3

16:2n-4 1.55 0.2 0.2

16:3n-3 <0.01 <0.1 0.1

16:4n-3 0.55 0.1 0.1

17:0 5.76 0.6 0.5

18:0 28.87 3.2 2.5

18:1n-11 3.33 0.4 0.5

18:1n-7 25.62 2.8 3.1

18:1n-9 92.99 10.2 8.4

18:2n-6 10.03 1.1 1

18:3n-3 6.47 0.7 0.8

18:3n-6 0.41 <0.1 0.1

18:4n-3 9.28 1 1.1


32


Name

2012-1421 Squid oil


NIFES

accumulated

profile for squid

oil

Fatty acid mg/g % %

20:0 2.13 0.2 0.2

20:1n-11 34.78 3.8 6.1

20:1n-7 2.99 0.3 0.4

20:1n-9 36.14 4 3.2

20:2n-6 4.61 0.5 0.4

20:3n-3 <0.01 <0.1 <0.1

20:3n-6 0.78 0.1 0.1

20:3n-9 <0.01 <0.1 <0.1

20:4n-3 5.06 0.6 0.7

20:4n-6 17.23 1.9 1.8

20:5n-3 EPA 91.12 10 12.2

21:5n-3 3.69 0.4 0.5

22:0 1.33 0.1 0.1

22:1n-11 42.87 4.7 5.9

22:1n-9 5.7 0.6 0.6

22:4n-6 1.44 0.2 0.2

22:5n-3 10.93 1.2 1.1

22:5n-6 5.46 0.6 0.4

22:6n-3 DHA 214.01 23.5 20.2

24:0 1.61 0.2 <0. 1

24:1n-9 7.38 0.8 0.7

24:5n-3 0.75 <0.1 <0.1


33


Name

2012-1421 Squid oil


NIFES

accumulated

profile for squid

oil

Fatty acid mg/g % %

24:6n-3 1.28 0.1 0.1

n-3/n-62 8.6 8.6 9.3

Sum 16:1 29.4 3.2 3.3

Sum 18:1 122 13.4 12

Sum 20:1 73.9 8.1 9.6

Sum 22:1 48.6 5.3 6.5

Sum mono-unsaturated 282 30.9 31.5

Sum EPA + DHA 305 33.5 32.1

Sum All FA 910 100 100

Sum poly-unsaturated 385 42.3 40.8

Sum identified FA 872 95.8 94.1

Sum saturated FA 206 22.6 21.8

Sum n-3 343 37.7 37.1

Sum n-6 40 4.4 3.5

Sum un-identified 38 4.2 6

2 Ratio of amounts. Unlike the other values there is no unit of measurement.


34

Table 7. Sterol-composition for biological species authentication, mg/kg and relative amounts (%), n=1.

Name 2012-1421 Squid oil

NIFES accumulated

profile for squid oil

Sterol mg/kg % %

Cholesterol 30780 90.1 92.0

Brassicasterol 2491.1 7.3 5.8

Campesterol 585.3 1.7 1.5

Campestanol 7 0 0

Stigmasterol 51.2 0.1 0.2

Sitosterol 87 0.3 0.2

Sitostanol 138.6 0.4 0.3

Stigmasta-dienol 0 0 0

Stigmast-enol 0 0 0

d-7-avenasterol 23.4 0.1 0

Sum phytosterols 3383.5 9.9 8.0

Sum Cholesterols 30780 90.1 92.0

Sum total 34163.5 100 100


35

Table 8. Heavy metal composition. n=109. Sample As Cd Hg Pb

mg/kg ww mg/kg ww mg/kg ww mg/kg ww

2012-1770/1 China Squid 0.27 0.03 0.02 0.01

2012-1624/1 Canada "Clams" 1.00 0.04 0.002 0.01

2012-1772/1 Vietnam Barramundi 0.38 0.001 0.08 < 0.005

2012-1636/1 Vietnam Squid 4.40 0.16 0.01 0.01

2012-1773/1 Taiwan Squid 1.00 0.12 0.10 0.03

2012-262/1 Russia Greenland halibut 3.80 < 0.001 0.09 < 0.008

2012-1420/1 China Anglerfish 5.30 0.01 0.11 < 0.006

2012-1622/1 Thailand "Fish" 0.19 0.02 0.03 < 0.03

2012-1426/1 USA Lobster 3.40 0.26 0.09 0.03

2012-1652/1 Canada Lobster 3.30 0.13 0.04 0.01

2012-1653/1 Canada Lobster 4.00 0.51 0.05 0.01

2012-1824/1 Canada Lobster 5.40 0.13 0.04 < 0.006

2012-1871/1 Canada Lobster 3.90 0.07 0.04 0.01

2012-1881/1 Canada Lobster 7.40 0.02 0.07 0.01

2012-577/1 Russia Haddock 4.02 < 0.001 0.02 < 0.006

2012-718/1 Russia Haddock 5.92 < 0.001 0.03 0.01

2012-722/1 Russia Haddock 10.70 < 0.001 0.03 0.01

2012-1619/1 USA Scallop 0.83 0.04 0.01 < 0.004

2012-1620/1 USA Scallop 0.41 0.03 0.003 < 0.004

2012-1635/1 USA Scallop 1.10 0.02 0.01 0.01

2012-1774/1 NA Scallop 1.60 0.09 0.01 < 0.006

2012-1918/1 Canada Scallop 1.70 0.09 0.02 < 0.006

2012-1917/1 Canada Forcemeat product 2.10 0.12 0.04 0.17

2012-1655/1 Vietnam Crab 22.00 0.02 0.09 0.01

2012-1872/1 Peru Crab 18.00 0.08 0.05 0.01

2012-1920/1 Thailand Crab 0.35 0.15 0.03 0.10

2012-666/1 USA Crab 5.20 0.03 0.02 0.01

2012-1769/1 Thailand Halibut 1.70 0.002 0.06 < 0.008

2012-1423/1 South Africa Hake 1.60 0.002 0.10 < 0.005


36



2012-1818/1 Turkey/Norway Mackerel 2.20 0.01 0.03 < 0.01

2012-1648/1 Philippines Milkfish 0.39 0.004 0.003 < 0.01

2012-1411/1 Morocco Marine oil 0.05 < 0.005 < 0.005 < 0.03

2012-1421/1 South Korea Marine oil 14.00 1.70 < 0.004 0.07

2012-1639/1 Vietnam Pangasius 0.38 0.004 0.002 < 0.004

2012-1771/1 Vietnam Pangasius 0.25 0.01 0.004 < 0.008

2012-1182/1 Sri Lanka Parrotfish 1.18 0.004 0.03 < 0.007

2012-110/1 India Red snapper 2.79 0.004 0.13 < 0.007

2012-538/1 Thailand Prawns 8.47 0.13 0.02 0.44

2012-1424/1 Canada Prawns 3.10 0.02 0.03 0.007

2012-1792/1 Canada Prawns 9.40 0.27 0.04 < 0.006

2012-1793/1 Canada Prawns 10.00 0.25 0.05 < 0.006

2012-1794/1 Canada Prawns 13.00 0.18 0.05 0.02

2012-1808/1 Canada Prawns 1.50 0.01 0.02 < 0.005

2012-1811/1 Canada Prawns 1.30 0.02 0.06 < 0.005

2012-1890/1 Canada Prawns 7.30 0.24 0.06 < 0.007

2012-194/1 Russia n.a. 0.96 < 0.001 0.005 < 0.008

2012-1657/1 Morocco Sardines 1.40 0.07 0.01 0.02

2012-1621/1 Vietnam Scampi 0.49 0.002 0.01 0.00

2012-1634/1 Vietnam Scampi 0.80 0.002 0.01 0.01

2012-1638/1 Vietnam Scampi 0.94 0.003 0.01 0.01

2012-1767/1 Thailand Scampi 0.08 0.01 0.01 < 0.01

2012-1807/1 Vietnam Scampi 0.25 0.003 0.01 < 0.004

2012-1885/1 Vietnam Scampi 0.53 0.003 0.01 < 0.005

2012-1905/1 Vietnam Scampi 0.53 0.002 0.01 0.01

2012-564/1 Russia Pollock 1.81 0.002 0.10 < 0.006

2012-569/1 Russia Pollock 3.10 < 0.001 0.03 < 0.006

2012-720/1 Russia Pollock 2.86 < 0.001 0.06 < 0.006

2012-1193/1 Russia Pollock 5.56 0.002 0.03 < 0.007


37



2012-1884/1 China Pollock 5.20 < 0.0008 0.06 < 0.005

2012-1627/1 Taiwan Mixed product 0.27 0.03 0.02 0.01

2012-1625/1 Thailand Mixed product 0.81 0.04 0.01 0.08

2012-1658/1 Thailand Forcemeat product 1.60 0.06 0.01 0.30

2012-1817/1 Thailand Forcemeat product 0.14 0.01 0.02 < 0.007

2012-1880/1 Vietnam Mixed product 0.10 0.004 < 0.002 < 0.01

2012-1882/1 Thailand Forcemeat product 0.50 0.05 0.10 < 0.03



2012-565/1 Russia Catfish 4.62 0.01 0.06 < 0.006

2012-1813/1 Thailand Catfish 1.40 0.13 0.02 0.05

2012-466/1 Sri Lanka Swordfish 0.71 0.04 0.24 < 0.006

2012-1797/1 Sri Lanka Swordfish 1.40 0.07 0.78 < 0.007

2012-1816/1 Kina Tilapia 0.34 < 0.001 0.01 < 0.007

2012-259/1 Russia Cod 1.00 < 0.001 0.01 < 0.008

2012-260/1 Russia Cod 1.26 0.001 0.01 < 0.008

2012-261/1 Russia Cod 1.07 < 0.001 0.01 < 0.008

2012-465/1 Russia Cod 0.79 0.002 0.00 < 0.006

2012-473/1 Greenland Cod 4.26 < 0.001 0.04 < 0.006

2012-521/1 China Cod 3.16 0.001 0.04 < 0.005

2012-522/1 China Cod 4.44 0.001 0.03 < 0.005

2012-535/1 China Cod 3.05 < 0.0006 0.01 < 0.004

2012-567/1 Russia Cod 2.44 < 0.0009 0.02 < 0.005

2012-719/1 Russia Cod 1.84 0.002 0.04 0.04

2012-721/1 Russia Cod 15.00 < 0.001 0.05 < 0.006

2012-726/1 Russia Cod 8.00 < 0.0009 0.03 < 0.005

2012-727/1 Russia Cod 15.70 < 0.0009 0.03 < 0.005

2012-728/1 Russia Cod 27.10 < 0.0009 0.03 < 0.005

2012-729/1 Russia Cod 14.20 < 0.0009 0.03 < 0.005


38



2012-730/1 Russia Cod 3.47 < 0.0007 0.02 < 0.004

2012-1080/1 Russia Cod 1.18 0.002 0.003 < 0.008

2012-1419/1 China Cod 4.70 0.001 0.02 < 0.006

2012-1425/1 China Cod 1.60 0.003 0.05 < 0.006

2012-1809/1 China Cod 0.97 0.001 0.06 < 0.005

2012-1883/1 China Cod 0.81 < 0.0006 0.03 < 0.004

2012-534/1 China Cod 2.05 < 0.0009 0.04 < 0.005

2012-467/1 Japan Tuna 1.01 < 0.002 0.17 < 0.01

2012-1181/1 Sri Lanka Tuna 1.32 0.02 0.54 < 0.008

2012-1819/1 Sri Lanka Tuna 0.88 0.01 0.25 < 0.008

2012-1820/1 Vietnam Tuna 1.50 0.01 0.20 < 0.008

2012-464/1 Russia Redfish 5.28 0.003 0.06 < 0.008

2012-536/1 China Redfish 1.02 0.003 0.06 0.01

2012-568/1 Russia Redfish 2.58 0.001 0.05 < 0.007

2012-1408/1 Russia Redfish 2.20 0.002 0.03 < 0.008

2012-1775/1 Vietnam "Fish" 0.91 0.02 0.03 < 0.03

2012-1295/1 Japan Yellowtail 1.39 < 0.002 0.11 < 0.01

2012-1823/1 Japan Yellowtail 0.76 0.002 0.14 < 0.01

2012-1649/1 Peru Trout 0.60 < 0.002 0.01 < 0.009

2012-1650/1 Peru Trout 0.44 < 0.001 0.02 < 0.008

2012-542/1 South Korea Oyster 2.16 0.49 0.01 0.10

2012-1623/1 Thailand Eel 0.19 0.002 0.09 0.02

# Of measurements 109 109 109 109

# of measureable values 109 82 106 36

Max value 27.1 1.7 0.78 0.4


39

Table 9. Dioxins and dioxin like PCBs. n=31. MO and NO means mono orto and non-orto. TE means Toxic equivalents.

Journal Nr.

Imported from

Group Species Tissue MO-PCB NO-PCB Sum

DLPCBs

Sum dioxins: PCDD/DF

Sum Total TE

Non-compliant

pg/g TE w.w pg/g TE w.w pg/g TE w.w pg/g TE w.w pg/g TE w.w NC

2012-96/1 Russia Marine fish Redfish Fillet 0.17 1.89 2.06 1.23 3.29 -

2012-194/1 Russia Marine fish Cod Roe 0.01 0.11 0.12 0.07 0.20 -

2012-262/1 Russia Marine fish Greenland Halibut

Fillet 0.10 1.30 1.40 1.01 2.41 -

2012-464/1 Russia Marine fish Redfish Whole gutted 0.03 0.39 0.42 0.36 0.79 -

2012-465/1 Russia Marine fish Cod Roe 0.01 0.09 0.10 0.06 0.16 -

2012-466/1 Sri Lanka Marine fish Swordfish Fillet 0.00 0.03 0.03 0.07 0.11 -

2012-467/1 Japan Marine fish Tuna Fillet 0.04 0.64 0.68 0.44 1.12 -

2012-490/1 Chile Marine oil n.a. Oil 0.04 0.75 0.79 2.06 2.85 -

2012-491/1 Peru Marine oil Oil Fish oil 0.03 0.82 0.85 1.49 2.34 -

2012-532/1 USA Marine oil Pollock Oil 0.07 0.63 0.70 1.22 1.92 -


Fillet 0.11 1.39 1.50 0.95 2.45 -

2012-566/1 Russia Marine fish Halibut Fillet 0.06 0.79 0.85 0.35 1.20 -

2012-619/1 Morocco Marine oil Oil Fish oil 0.05 1.18 1.23 1.49 2.73 -


Fillet 0.06 0.63 0.69 0.32 1.01 -

2012-1181/1 Sri Lanka Marine fish Tuna Fillet 0.00 0.01 0.01 0.02 0.03 -

2012-1182/1 Sri Lanka Marine fish Parrotfish Whole 0.00 0.00 0.01 0.02 0.02 -

2012-1295/1 Japan Marine fish Yellowtail Fillet 0.08 1.07 1.15 0.56 1.71 -


40

Table 9. Dioxins and dioxin like PCBs. n=31. MO and NO means mono orto and non-orto. TE means Toxic equivalents.

Journal Nr.

Imported from

Group Species Tissue MO-PCB NO-PCB Sum

DLPCBs

Sum dioxins: PCDD/DF

Sum Total TE

Non-compliant

2012-1408/1 Russia Marine fish Redfish Whole gutted 0.03 0.33 0.35 0.28 0.63 -

2012-1411/1 Morocco Marine fish Sardines Oil 0.05 0.41 0.47 0.58 1.05 -

2012-1420/1 China Marine fish Anglerfish Fillet 0.00 0.01 0.01 0.01 0.02 -

2012-1421/1 South Korea Cephalopod Squid oil 0.88 26.1 26.9 14.1 41.0 NC

2012-1454/1 USA Marine oil n.a. Fish oil 0.82 2.96 3.77 1.22 5.00 -

2012-1622/1 Thailand Marine fish "marine fish"

Minced fish product

0.00 0.02 0.03 0.20 0.23 -

2012-1623/1 Thailand Marine fish Eel Fillet 0.01 0.33 0.34 0.42 0.76 -

2012-1636/1 Vietnam Cephalopod Squid whole 0.00 0.01 0.01 0.04 0.05 -

2012-1639/1 Vietnam Marine fish Pangasius Fillet 0.00 0.00 0.00 0.03 0.03 -

2012-1648/1 Philippines Marine fish Milkfish Fillet 0.00 0.05 0.05 0.09 0.14 -

2012-1649/1 Peru Marine fish Trout Fillet 0.00 0.05 0.06 0.14 0.20 -

2012-1650/1 Peru Marine fish Trout Fillet 0.00 0.04 0.05 0.06 0.10 -

2012-1657/1 Morocco Marine fish Sardines Sardines in oil 0.01 0.04 0.05 0.15 0.20 -

2012-1818/1 Turkey/ Norway

Marine fish Mackerel Fillet 0.03 0.31 0.34 0.19 0.53 -

Max 0.88 26.1 26.9 14.1 41.0


41

3 PCB-118 is not part of the sum 6-PCBs. It was part of the sum 7-PCBs (ICES-7). For backward compatibility it may still be of interest as an indicator compound.

Table 10. Levels of indicator PCBs (µg/kg w.w.). Sum 6-PCB calculated as upper bound sum, n=4.


from Group Species Tissue

PCB

28

PCB

52

PCB

101

PCB

1183

PCB

138

PCB

153

PCB

180

Sum

6-PCB

2012-1920/1 Thailand Crustacean Crab White + brown meat

0.01 0.02 0.005 0.01 0.01 0.01 0.01 0.07

2012-1951/1 Norway/ USA Marine oil Oil Oil 1 1 0.4 1.6 4.1 3.9 1.8 12.2

2012-1797/1 Sri Lanka Marine fish Swordfish Fillet 0.05 0.1 0.017 0.02 0.05 0.06 0.03 0.2

2012-1819/1 Sri Lanka Marine fish Tuna Fillet 0.1 0.1 0.05 0.04 0.04 0.04 0.03 0.4

Max. 1 1 0.4 1.6 4.1 3.9 1.8 12.2


42

4 PBDE-66 is not included in the sum 7PBDE.

Table 11. Levels of PBDEs (µg/kg w.w.). Sum 7-PBDE calculated as upper bound sum. n=29, n.a.=”not available”


from Group Species Tissue

PBDE-100

PBDE-153

PBDE-154 PBDE-

183 PBDE-

28 PBDE-

47 PBDE-

664 PBDE-99

Sum 7-

PBDE

2012-96/1 Russia Marine fish Redfish Fillet 0.15 0.03 0.21 < 0.005 0.04 1.3 0.01 0.01 1.7

2012-194/1 Russia Marine fish cod Roe 0.005 < 0.002 0.004 < 0.004 0.006 0.04 < 0.002 < 0.004 0.06

2012-262/1 Russia Marine fish Greenland

Halibut Fillet 0.11 0.02 0.09 < 0.007 0.07 0.84 0.03 0.02 1.2

2012-464/1 Russia Marine fish Redfish Whole 0.05 0.006 0.03 < 0.001 0.01 0.3 0.004 0.007 0.4

2012-465/1 Russia Marine fish Cod Roe 0.004 < 0.001 0.003 < 0.002 0.004 0.03 < 0.001 < 0.002 0.04

2012-466/1 Sri Lanka Marine fish swordfish Fillet < 0.002 < 0.002 0.004 < 0.005 < 0.002 0.006 < 0.002 < 0.005 0.01

2012-467/1 Japan Marine fish Tuna Fillet 0.06 0.02 0.06 < 0.009 0.04 0.36 0.05 0.04 0.58

2012-490/1 Chile Marine oil n.a. Fish oil < 0.04 < 0.04 0.04 < 0.08 < 0.04 0.59 < 0.04 < 0.08 0.63

2012-491/1 Peru Marine oil n.a. Fish oil < 0.04 < 0.04 < 0.04 < 0.07 < 0.04 0.28 < 0.04 < 0.07 0.28

2012-532/1 USA Marine fish Pollock Fish oil < 0.04 < 0.04 < 0.04 < 0.09 0.06 0.25 < 0.04 < 0.09 0.31


Halibut Fillet 0.1 < 0.01 0.09 < 0.02 0.04 0.76 0.02 0.04 1

2012-566/1 Russia Marine fish Halibut Fillet 0.11 0.02 0.12 < 0.004 0.02 0.6 0.02 0.02 0.89

2012-619/1 Morocco Marine oil n.a. Fish oil < 0.04 < 0.04 < 0.04 < 0.09 < 0.04 0.26 < 0.04 < 0.09 0.26


Halibut Fillet 0.06 0.005 0.06 < 0.008 0.02 0.4 0.01 0.01 0.6

2012-1181/1 Sri Lanka Marine fish Tuna Fillet < 0.002 < 0.002 < 0.002 < 0.003 < 0.002 < 0.003 < 0.002 < 0.003 -

2012-1182/1 Sri Lanka Marine fish Parrotfish Fillet < 0.001 < 0.001 < 0.001 < 0.003 < 0.001 < 0.003 < 0.001 < 0.003 -


43

2012-1295/1 Japan Marine fish Yellowtail Fillet 0.1 0.03 0.11 < 0.02 0.08 0.5 0.05 0.07 0.89

2012-1408/1 Russia Marine fish Redfish Whole 0.03 0.004 0.04 < 0.003 0.008 0.19 0.002 0.005 0.28

2012-1411/1 Morocco Marine oil n.a. Oil 0.05 < 0.04 < 0.04 < 0.08 < 0.04 0.35 < 0.04 0.08 0.48

2012-1420/1 China Marine fish Anglerfish Fillet < 0.001 < 0.001 < 0.001 < 0.002 < 0.001 < 0.002 < 0.001 < 0.002 -

2012-1421/1 South Korea Cephalopod Cuttlefish Marine oil 1.3 0.66 2.9 < 0.08 0.28 6.9 0.59 1.8 14

2012-1454/1 USA n.a. n.a. Marine oil 4.1 0.36 1.2 < 0.08 1.4 25 0.3 0.62 33

2012-1622/1 Thailand n.a. n.a. "Fish snacks" < 0.006 < 0.006 < 0.006 < 0.01 < 0.006 < 0.01 < 0.006 < 0.01 -

2012-1623/1 Thailand Marine fish Eel Fillet 0.02 < 0.006 0.03 < 0.01 < 0.006 0.1 < 0.006 < 0.01 0.2

2012-1636/1 Vietnam Cephalopod Cuttlefish Whole < 0.0009 < 0.0009 < 0.0009 < 0.002 < 0.0009 0.002 < 0.0009 < 0.002 0.002

2012-1639/1 Vietnam Freshwater

fish Pangasius Fillet 0.0008 < 0.0007 < 0.0007 < 0.001 < 0.0007 0.004 < 0.0007 0.006 0.01

2012-1648/1 Philippines Marine fish Milkfish Fillet 0.005 0.003 0.01 < 0.004 < 0.002 0.03 < 0.002 < 0.004 0.05

2012-1657/1 Morocco Marine fish Sardines Decapitated < 0.005 < 0.005 < 0.005 < 0.01 < 0.005 0.02 < 0.005 < 0.01 0.02

2012-1818/1 Turkey/Norway Marine fish Mackerel Fillet 0.08 0.02 0.04 < 0.01 0.02 0.3 0.04 0.1 0.6

Max 4.1 0.66 2.9 <LOQ 1.4 25 0.6 1.8 33


44

Table 12. Maximum levels of pesticides (µg/kg w.w.) n=23

Group Marine fish Freshwater fish Cephalopod Marine oil

Total

Tissue Fillet Fillet Fillet Oil

Samples n=14 n=1 n=1 n=6 n=22

Pesticide Max value

N

Max value Max value Max value n

Max value

Aldrin 4.8 14 <0.22 <0.22 <0.6 4.8

Hexachlorhexane HCH-alfa

1.5 14 <0.04 0.05 2.4 6 2.4

Hexachlorhexane HCH-beta

0.82 7 0.15 0.39 6.1 3 6.1

Hexachlorhexane HCH-delta

0.08 7 0.1 <0.04 <0.1 3 0.08

Hexachlorhexane HCH-gamma

0.59 14 0.18 <0.1 2.1 6 2.1

Cis-chlordane 5.2 13 <0.04 <0.04 14 6 14

Trans-chlordane 1.2 14 <0.04 <0.04 5.2 6 5.2

Oxy-chlordane 1.2 14 <0.04 <0.04 1.5 6 1.5

Dieldrin 3.2 14 0.10 0.05 29 6 29

Endrin 0.44 7 <0.04 0.10 1.8 3 1.8

Endosulfane-alfa 1.4 14 <0.2 <0.2 <0.5 6 1.4

Endosulfane-beta 1.2 14 <0.4 <0.4 <0.9 6 1.2

Endosulfane-Sulfate 2.6 14 <0.4 <0.4 1.7 6 2.6

Hexachlorobenzene HCB

7.8 14 1.9 2.4 22 6 22

Pentachlorobenzene 0.48 14 <0.04 <0.04 1.9 6 1.9

Heptachlor 0.05 14 <0.2 <0.2 <0.5 6 0.05

Heptachlor cis epoxide 0.52 14 <0.04 <0.04 3.7 3 3.7

Heptachlor trans epoxide

0.34 14 <0.2 <0.2 1.3 6 1.3

Nonachlor-cis 0.32 7 - - <0.2 3 0.3

Nonachlor-trans 7.4 14 <0.04 <0.04 20 6 20

Isodrin <1 7 - - <5 3 <LOQ

Mirex 0.34 14 <0.04 <0.04 1.3 6 1.3


45

Octachlorstyrol 0.37 7 <0.04 <0.04 2.4 3 2.4

Toxaphene-26 5.1 14 <0.1 <0.1 3.8 6 5.1

Toxaphene-32 <0.4 7 - - <1 3 <LOQ

Toxaphene-42a 0.09 7 - - <0.4 3 0.09

Toxaphene-50 6.2 14 <0.2 <0.2 4.3 6 6.2

Toxaphene-62 2.5 12 <0.4 <0.4 2.8 6 2.8

o,p-DDD 1.8 14 <0.04 <0.04 19 6 19

o,p-DDE 0.58 14 <0.04 <0.04 4.3 6 4.3

o,p-DDT 1.3 14 <0.04 <0.04 2.9 6 2.9

p,p-DDD 8.2 14 0.1 <0.04 74 6 74

p,p-DDE 18 14 0.28 0.16 100 6 100

p,p-DDT 6.4 14 0.06 <0.04 11 6 11


46

Table 13. PAH maximum levels (µg/kg w.w.), n=23. (The compound with a legal limit is highlighted with colour.)

(PAH4 is the LB sum of BaP, BaA, BbF and chrysene) Group

Freshwater fish Cephalopod Bivalve Crusta- cean

Marine fish. Freshwater fish

LOQ Max value

Number of Non

compliant

Species

Marine oil Squid Scallop

and clam

Crab and Lobster

Monkfish Milkfish Redfish Wolffish

Yellowtail Pangasius

Tissue/Matrix Oil Whole Soft tissue

Brown meat. White meat

Fillet

Number of samples 5 1 5 3 9

5-Methylchrysene <LOQ <LOQ <LOQ <LOQ <LOQ 1 - -

Anthracene - - - <LOQ - 0.5 - -

Anthranthrene - - - <LOQ - 1 - -

Benzo(a)antracene (BaA) 1.0 <LOQ <LOQ <LOQ <LOQ 0.5 1.0 -

Benzo(a)pyrene (BaP) 1.3 <LOQ <LOQ <LOQ <LOQ <LOQ 1.3 0

Benzo(b)fluoranthene (BbF) 5.5 <LOQ 1.3 <LOQ <LOQ 0.5 5.5 -

Benzo(b)naphto(2.1-d)thiophene - - - <LOQ - 1 - -

Benzo(c)fluorene 1.9 <LOQ <LOQ <LOQ <LOQ 1 1.9 -

Benzo(e)pyrene - - - <LOQ - 1 - -

Benzo(ghi)perylene 1.3 <LOQ <LOQ <LOQ <LOQ 0.5 1.3 -

Benzo(j)fluoranthene 3.2 <LOQ <LOQ <LOQ <LOQ 0.5 3.2 -

Benzo(k)fluoranthene 2.9 <LOQ 0.8 <LOQ <LOQ 0.5 2.9 -

Chrysene 49 <LOQ 0.7 <LOQ <LOQ 0.5 49 -

Coronene - - - <LOQ - 1 - -

Cyclopenta(c.d)pyrene 48 <LOQ <LOQ <LOQ <LOQ 1 48 -

Dibenzo(a.e)pyrene <LOQ <LOQ <LOQ <LOQ <LOQ 1 - -

Dibenzo(a.h)anthracene <LOQ <LOQ <LOQ <LOQ <LOQ 1 - -

Dibenzo(a.h)pyrene <LOQ <LOQ <LOQ <LOQ <LOQ 1 - -

Dibenzo(a.i)pyrene <LOQ <LOQ <LOQ <LOQ <LOQ 1 - -

Fluoranthene - - - 1.0 - 0.5 1.0 -

Fluorene <LOQ <LOQ <LOQ <LOQ <LOQ 0.5 - -

Indeno(1.2.3-cd)pyrene 1.4 <LOQ 0.5 <LOQ <LOQ 0.5 1.4 -

Perylene - - - <LOQ - 1 - -

Phenantrene - - - 1.2 - 0.5 1.2 -

Pyrene - - - 0.53 - 0.5 0.53 -

Max PAH4 in one sample 120 0 2.8 2.7 0 - 120 -

Maximum LB 4-SUM PAH 56 0 1.0 1


47

Table 14. A summary of maximum levels for some contaminants in foodstuffs.

Element or

pollutant

Unit of

measur

ement

Marin Fish

Muscle

Some fish

species

muscle

Eel

Muscle

Fresh

water

Fish

Muscle

Smoked

seafood

products

Fish

liver

Crustace

ans

Bivalves

and

(smoked

bivalves)

Cephalo

pods

Marine

oils

and

fats

Arsenic (As)

- - - - - - - - -

Cadmium (Cd) Mg/kg

w.w. 0.05 0.1-0.3 0.1 0.05 - - 0.5 1.0 1.0 -

Mercury (Hg)

0.5 1 1.0 0.5 0.5 - 0.5 0.5 - -

Lead (Pb)

0.3 0.3 0.3 0.3 0.3 - 0.5 1.5 1.0 -

Sum of dioxins

and furans

Pg/g

TEQ

w.w.

3.5 3.5 3.5 - - - - - 1.75

Sum of dioxin

like PCBs - - - - - - - -

Sum of dioxins.

furans and

dioxin like PCBs

6.5 10 10 - 20 - - - 6

Sum of six

indicator PCBs

Ng/g

w.w. 75 300 125 - 200 - - - 200

PAH

Benzo[a]pyrene

μg/kg

w.w

- - - 52 - - 5

(6)1 - 2

PAH4, the sum of

4 compounds

μg/kg

w.w. - - - 302 - -

30

(35) - 10

1) Value in brackets concerns smoked bivalves.

2) Valid until 2014. It is then reduced to a smaller value.

ANNEX 2: TABLE 14 A Summary of maximum levels


48

Table 15. Summary of chemical analytical methods.

Compounds

Matrix Method

principle

Screening

method

LOD

wet weight

(µg/kg w.w.)

Analytical

method

LOD

in muscle)

(µg/kg w.w.)*)

Analytical

method

LOQ

wet weight

(µg/kg w.w.)

Level of action Laboratory

Therapeutic agents

and dyes

Chloramphenicol Muscle LC-MS n.a. 0.25

1.0

presence (MRPL=0.3)

NIFES

3-Amino-2-oxazolidinone

(AOZ) Muscle LC-MS/MS n.a.

0.2

0.5

presence (MRPL=1.0)

Eurofins

1-Aminohydrantoin

(AHD) Muscle LC-MS/MS n.a. 0.3 1.0

presence (MRPL=1.0)

Eurofins

3-Amino-5-morpholinomethyl-

2-oxazolidinone (AMOZ) Muscle LC-MS/MS n.a. 0.2 0.5

presence (MRPL=1.0)

Eurofins

Semicarbazide

(SEM) Muscle LC-MS/MS n.a. 0.3) 1.0

presence (MRPL=1.0)

Eurofins

Malachite green

(MG) Muscle LC-MS/MS n.a.

0.15

0.5

presence (MRPL=2.0)

NIFES

Leuco malachite green

(LMG) Muscle LC-MS/MS n.a.

0.15

0.5

presence (MRPL=2.0)

NIFES

Crystal violet

(CV) Muscle LC-MS/MS n.a. 0.3 1.0 Presence NIFES

Leuco crystal violet

(LCV) Muscle LC-MS/MS n.a. 0.15 0.5 Presence NIFES

Brilliant green

(BG) Muscle LC-MS/MS n.a. 0.15 0.5 Presence NIFES

Organochlorine

compounds

PCDD and PCDF

(dioxins and furans) Muscle GC-HRMS n.a.

0.003-0.01

ng/kg

0.01-0.03

ng/kg See table 14 NIFES

non- and mono-orto PCB Muscle GC-HRMS n.a. 0.01-2

ng/kg

0.03-6

ng/kg See table 14 NIFES

PCB-28 Muscle GC-MS n.a. 0.005-0.03 0.03-0.1 n.a. NIFES




ANNEX 3: Table 15 Method performance data


49


Compounds

Matrix Method

principle

Screening

method

LOD

wet weight

(µg/kg w.w.)

Analytical

method

LOD

in muscle)

(µg/kg w.w.)*)

Analytical

method

LOQ

wet weight

(µg/kg w.w.)





HCH-alfa Muscle GC-MS n.a. 0.01-0.2 0.03-0.6 n.a. NIFES

HCH-beta Muscle GC-MS n.a. 0.01-0.04 0.03-0.1 n.a. NIFES

HCH-delta Muscle GC-MS n.a. 0.01-0.04 0.03-0.1

HCH-gamma Muscle GC-MS n.a. 0.03-0.2 0.1-0.6 n.a. NIFES

Hexachlorobenzene Muscle GC-MS n.a. 0.01-0.06 0.05-0.2 n.a. NIFES

Pentachlorobenzene Muscle GC-MS n.a. 0.02-0.05 0.05-1.0 n.a. NIFES

Heptachlor Muscle GC-MS n.a. 0.01-0.1 0.02-0.4 n.a. NIFES

Heptachlor-cis-epoxide Muscle GC-MS n.a. 0.02 0.05 n.a. NIFES

Heptachlor-trans-epoxide Muscle GC-MS n.a. 0.01-0.1 0.02-0.4 n.a. NIFES

Aldrin Muscle GC-MS n.a. 0.01-0.2 0.03-0.6 n.a. NIFES

Isodrin Muscle GC-MS n.a 0.01-0.6 0.03-2 n.a NIFES

Dieldrin Muscle GC-MS n.a 0.02 0.04-0.05 n.a NIFES

Endrin Muscle GC-MS n.a 0.02 0.05 n.a NIFES

Oxy-chlordane Muscle GC-MS n.a. 0.01-0.2 0.03-0.4 n.a. NIFES

trans-Chlordane Muscle GC-MS n.a. 0.02-0.1 0.05-0.2 n.a. NIFES

cis-Chlordane Muscle GC-MS n.a. 0.02-0.2 0.05-0.6 n.a. NIFES

Alfa-endosulfan Muscle GC-MS n.a. 0.01-0.2 0.03-0.4 n.a. NIFES

Endosulfan-sulphate Muscle GC-MS n.a. 0.01-0.2 0.02-0.4 n.a. NIFES

Beta-endosulfan Muscle GC-MS n.a. 0.01-0.2 0.02-0.4 n.a. NIFES

cis-Nonachlor Muscle GC-MS n.a. 0.02-0.04 0.04-0.2 n.a. NIFES

trans-Nonachlor Muscle GC-MS n.a. 0.02-0.04 0.04-0.4 n.a. NIFES


50


Compounds

Matrix Method

principle

Screening

method

LOD

wet weight

(µg/kg w.w.)

Analytical

method

LOD

in muscle)

(µg/kg w.w.)*)

Analytical

method

LOQ

wet weight

(µg/kg w.w.)


Mirex Muscle GC-MS n.a. 0.01-0.2 0.03-0.6 n.a. NIFES

Toxaphene 26 Muscle GC-MS n.a. 0.02-0.2 0.05-0.6 n.a. NIFES





Sum Toxaphene 40+41 Muscle GC-MS n.a. 0.02-0.2 0.05-0.6 n.a. NIFES

OctaChlorstyrol Muscle GC-MS n.a. 0.02-0.04 0.05-0.1 n.a. NIFES

o,p-DDT

p,p-DDT

o,p-DDD

p,p-DDD

o,p-DDE

p,p-DDE

Muscle GC-MS n.a. 0.01-1.0 0.04-3.0 n.a. NIFES

PBDE-congeners:

PBDE-28

PBDE-47

PBDE-66

PBDE-99

PBDE-100

PBDE-119

PBDE-138

PBDE-153

PBDE-154

PBDE-183

Muscle GC-MS n.a. 0.001-0.003 0.002-0.006 n.a. NIFES

Chemical elements

Pb Muscle ICPMS n.a. 0.004 0.01 See table 14

NIFES

Cd Muscle ICPMS n.a. 0.004 0.01 See table 14

NIFES

As Muscle ICPMS n.a. 0.004 0.01 See table 14

NIFES

Hg Muscle ICPMS n.a. 0.004 0.01 See table 14

NIFES


51


Compounds

Matrix Method

principle

Screening

method

LOD

wet weight

(µg/kg w.w.)

Analytical

method

LOD

in muscle)

(µg/kg w.w.)*)

Analytical

method

LOQ

wet weight

(µg/kg w.w.)


Combustion by-

products

PAH,

benzo(a)pyrene(BaP)

SUM 4PAH

Muscle GC-MS n.a. 0.1-0.3 0.5-1.0 See table 14 sub contractor

veterinær grensekontrollrapport 2012

Documents

veterinary control

monitoring programme

fisheries products

seafood products

chemical analysis

analytical work

rapport monitoring program

day technical work