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Microsoft word - qbe8f.docControl of Residues in Live Animals and Animal Products. Results 2005, plan 2006. Originating from the Faroe Islands (FO), Pursuant to Council Directive 96/23/EC. PRESENTATION OF THE
RESIDUE CONTROL 2005
RESIDUE CONTROL PLAN 2006
Date: 30th March 2006
Commission Reference Number (Stamp):
2005 and Plan for 2006
Animal/Products Covered in the Present Plan:
Faroese Food-, Veterinary and Environmental Agency
Óluva Niclasen, Head of Department
FVEA file 20050022-46 1. General Information Table of Contents GENERAL INFORMATION. 4
1.1 Legislation Concerning the Use of Substances in Annex I. 4
1.2 Infrastructure of Official Services; Information on Co-ordination of Activities of
Central and Regional Departments . 5 1.3 National Tolerance Limits (MRL´s) for Authorised Substances and Environmental 1.4 Official Sampling Procedure in the Field, Including Information on How Samples Are Secured After Collection. 6 1.4.1 Sampling LIST OF OFFICIAL LABORATORIES. 8
2.1 Level of Competence of the National Reference Laboratory . 9
2.2 Details of Analysis Methods - Screening /Routine and Confirmation, with Action
Levels and Detection Limits . 9 2.2.1 Screening of Stilbenes and Steroides in Fish. 10 Confirmation of Stilbenes and Steroides in Fish . 10 Screening test for the detection of Chloramphenicol in Fish muscle by ELISA . 10 B 1 Antibacterial substances. 10 Screening for Ivermectin ans Emamectin in Salmon by LC/FLUORESCENCE . 10 Determination of PCBs, Organochlorine and Pyrethorid pestiside residues in fish . 10 Analytical methods for Organochloriniated pesticides and toxaphenénes congeners. 11 Analytical methods for PCDD's/PCDF's . 11 2.2.9 WHO-PCBs. 12 2.2.10 Marker-PCBs . 13 2.2.11 Methods used in determining Pb, Cd and Hg in salmon. 13 2.2.12 Malachite 2.2.13 Cantaxathin . 14 2.2.14 Screening and Confirmation of Mycotoxin . 14 NATIONAL TOLERANCES FOR SUBSTANCES . 16
3.1 Description of Measures Taken by Competent Authorities When Residues Are
Detected. 16 3.1.1 Category A Substances: . 16 Category B1 Substances: . 16 SCOPE OF THE RESIDUE PLAN . 17
4.1 Group of Residues Covered . 17
The following changes have been made from the previous report: . 17 The category A, substances: . 17 4.1.3 Sulfonamides. 17 RESIDUES PLAN FOR THE EXAMINATION IN AQUACULTURE PRODUCTS
2006 . 20
BACKGROUND INFORMATION ON PRODUCTION. 22
6.1 Animal Species and Total Figures of Production . 22
1. General Information 6.1.2 Production 6.2 Type of Production. 22 FREQUENCIES AND LEVELS OF THE CONTROLS . 23
7.1 Number of samples . 23
TARGETING CRITERIA. 24
8.1 Changes Based on Analyses of the Residue Plan of the Previous Years. 24
OVERVIEW OF TABLES
Table 1. Internal Standards (13C-UL), PCDDs/PCDFs .11
Table 2. The following PCDDs/PCDFs are reported.11
Table 3. Internal standards (13C-UL), WHO-PCBs .12
Table 4. WHO-PCBs.12
Table 5. Limit of Detection.14
Table 6. Results 2005, Group A.17
Table 7. Results 2005, Group B.18
Table 8. Annual plan for the examination for residues, Group A.20
Table 9. Annual plan for the examination for residues, Group B, and Totals .21
Table 10. Exports in Aquaculture Products from the Faroe Islands .22
OVERVIEW OF APPENDIX (attachment)
1. Register of stock farmes
2. Register of approved processing plants
3. Quality control for The Laboratory at ERGO.
4. Accreditation Certificate for the National Food-, Veterinary- and Environmental Agency.
5. Detailed results.
6. Division of samples among stock farms.
7. Check table
8. The survey of used medicines in 2004 and 2005.
1. General Information General Information
1.1 Legislation Concerning the Use of Substances in Annex I
Article 7, point 1, pursuant to Council Directive 96/23/EC.
The legislation regarding the use of pharmaceuticals is stipulated in the Parliamentary Act
Governing the National Pharmacy Service and Medicinal Products, Act No. 54 from 1991, and the
Parliamentary Act Governing Food, Act No. 46 from 1985.
The Parliamentary Act Governing the National Pharmacy Service and Medicinal Products ensure
that only registered and/or approved pharmaceuticals (hereinafter, "medicines") may be imported
into the Faroe Islands. All said medicines shall be dispensed through the National Pharmacy
Service, which is a public, administrative authority regulated by the above-named authorising
legislation. The National Pharmacy Service utilizes the services of the Faroese Customs and Tax
Administration to assist in the control of the importation of medicines. The National Pharmacy
Service controls the monopoly for both the importation and the dispensing of prescribed medicines.
The use of said medicines is not only controlled by the Parliamentary Act Governing the National
Pharmacy Service and Medicinal Products, but also the Parliamentary Act Governing the National
Veterinary Service. Only authorised veterinarians may write prescriptions for medicines. Currently,
only two licensed fisheries veterinarians work within the aquaculture industry in the Faroe Islands.
The National Pharmacy Service may only dispense medicines prescribed by licensed veterinarians.
The Chief Veterinary Officer receives a copy of all prescriptions, and is able, therefore, to monitor
the various stock farms in the Faroe Islands.
The Chief Medical Officer, the Chief Veterinary Officer, and the Chief Pharmaceutical Officer
approve the various types of medicines that are used in fish farming and stipulate the withdrawal
time before harvest for the various medicines. Medicines that are not approved for fish farming may
not be used.
The National Food-, Veterinary-, and Environmental Agency (FVEA) receives a report, or copies of
the prescriptions, issued from the veterinarians, and are sent notices about harvesting of fish from
the factories. The factories are responsible for their own checks and for accepting only animals for
which the producer is able to guarantee that withdrawal times have been observed.
All stock farms are registered with the Agricultural Agency,
http://www.bunadarstovan.fo/pub/index.php?id=45 (see attachment 1).
They are subject to Parliamentary Act no.16, from 23 February 2001, concerning animal diseases,
prevention and combating diseases in animals and market supervision of animals and animal
extracts and the environmental protection laws, which the National Food-, Veterinary- and
Environmental Agency administers.
Moreover, pursuant to the Faroese Food Act (Act No. 46 from 1985), the National Food-,
Veterinary- and Environmental Agency conducts regular inspections of all fish processing plants in
the Faroe Islands. All fish processing plant are approved according to directive 91/493,
http://www.hfs.fo (see attachment 2).
1. General Information The fish processing plants label the packages of their products in compliance with labelling
regulations so that the contents can be traced back not only to the fish processing plant, but also to
the originating stock farm.
1.2 Infrastructure of Official Services; Information on Co-ordination of Activities of
Central and Regional Departments
Article 7, point 3, pursuant to Council Directive 96/23/EC.
CHIEF PHARMACEUTICAL OFFICER: See Attachment 1, in the residue control plan 2002,
dated 19th March 2002. (FEA file 401-200100175)
CHIEF VETERINARY OFFICER: See Attachment 2, in the residue control plan 2002, dated
19th March 2002. (FEA file 401-200100175)
NATIONAL FOOD, VETERINARY AND ENVIRONMENTAL AGENCY (FVEA):
According to the COMMISSION DECISION of 23 JULY 1993, based on 93/494/EØF, the FVEA
Food Department is approved by the EU as a competent inspection authority with respect to fish
The Food Department of FVEA employs four scientists, and six food and fish inspectors.
Inspections are made pursuant to the Faroese Food Act, which is similar to the former Danish Food
Act. See Attachment 3, in the residue control plan 2002, date 19th of March 2002. (FEA file 401-
The Fish Disease Department of FVEA employs 3 scientists, and 1 fish inspector.
Inspections are made pursuant to the Parliamentary Act no.16 from 23 February 2001; concerning
Animal diseases and Departmental order no. 131, from 23rd December 2003, concerning disease-
preventative operations on stock farms, and no. 130, from 23rd December 2003, concerning
prevention and control of Infectious Salmon Anaemia, ISA.
The FVEA is under the Faroese Ministry of Industry and Trade. The Chief Veterinary Officer is
part of the Ministry of Industry and Trade.
See also the decision No. 1/2001 of the EC-Faeroe Islands joint committee (2001/127/EF),
Attachment 4, in the residue control plan 2002, date 19th of March 2002. (FEA file 401-
1.3 National Tolerance Limits (MRL´s) for Authorised Substances and Environmental
Article 7, point 4, pursuant to Council Directive 96/23/EC. Detection limits are also tolerance limits for unauthorised types of veterinary medicinal products. For the authorised medicines, the Maximum residue limit (MRL) as defined in Annex I in Commission Regulation (EC) 2377/90 and later amendments, or, if such has not been defined, the provisional MRL, as defined in Annex III of the above-mentioned regulation, is regarded as the tolerance limit. For substances listed in Annex IV of the above-mentioned regulation, the detection of any residue is unacceptable. The tolerance limit for environmental pollutant is defined by the EU Decision 93/351/EEC. Heavy metal is defined in Commission Regulation (EC) No 78/2005 of 19 1. General Information January 2005, amending regulation (EC) No 466/2001 as regards heavy metals. Commission
Regulation (EC) No 199/2006 of 3 February 2006 amending Regulation (EC) No 466/2001 setting
maximum levels for certain contaminants in foodstuffs as regards dioxins and dioxin-like PCBs
For substances not embraced by the above-mentioned regulations and guidelines, a positive
detection will initiate an investigation and assessment of whether the findings needs to be
communicated to representatives of customers, or whether an action directed towards the producers
The detection limits using current analytical methods are shown in section 2.3.
If any samples are found to contain unacceptable residues of medicines or substances used in the
production, necessary corrective steps are taken immediately, both with respect to the fish from
which the sample was taken and the stock farm that raised the fish.
Corrective action is taken pursuant to §11 of the Food Act, which states:
It is not allowed to sell food for general use if it is suspected it will cause illness or poisoning, or if
the food, due to pathological changes, putrefaction, pollution, incorrect preparation or by other
means can [be] judged unfit for human consumption.
It should be noted that for medicines there have been no positive test results in the years 1987 –
There have been no reported incidences where the stipulated withdrawal times before harvest have
not been fulfilled. There have been no reported incidents of the use of unlawful substances.
1.4 Official Sampling Procedure in the Field, Including Information on How Samples Are
Secured After Collection
(Using Flow Charts) (Des 98/179/EC) Samples of fish and feed are collected in accordance with instructions given by National Food-, veterinary-, and Environmental Agency. Inspectors employed by FVEA, collect the samples from fish farms or processing plant. To comply with regulations governing inspections of stock farms and their use of medicines, inspectors from the National Food-, Veterinary- and Environmental Agency take samples as required. 1.4.1 Sampling Procedures The inspector visits the stock farm, accompanied by a representative from the stock farm. Fish are taken from the ring(s) that should be tested. Care is taken to obtain fish that do not appear to be diseased. The fish is, gutted. Or the inspector visits the processing plant, and takes a random sample of bled and beheaded fish and liver. Samples are taken from at least five fish from a designated ring. One sample consists of a small piece of each fish or its liver. Each test sample is placed in an impermeable plastic bag and well sealed. The sample bags are numbered 1, 2, 3, 4, 5, etc. Bagged samples of representative fish from the same ring are collected in one large plastic bag. 1. General Information This large plastic bag is labelled as follows: the test date, the name of the stock farm, the
registration number of the stock farm, the ring number, the sample number, the inspector's name,
the medicine(s) to be detected, i.e., oxitetracyclin: antibiotic.
The muscle and liver-samples are kept frozen at the laboratories until analysis. The feed is kept cool
Rules concerning collection of official samples are laid down.
2. List of Official Laboratories List of Official Laboratories
Article 7, point 3, pursuant to Council Directive 96/23/EC. 1. Official Laboratory: National Food, Veterinary and Environmental Agency (FVEA), Microbiological and Chemical Laboratory, is used for B 1 Antibacterial substances and B 3c Chemical elements. Drug Residue Testing Capacity: Antibacterial substances are detected by plate method 6-G001, sensitive to sulphonamides, tetracyclines, florfenikol, oxolinic acid, quinolones and flumequin. When residues are detected, samples are forwarded to the Danish Food Directorate, Institute for Food Product Testing and Nutrition, for verification and identification. 2. At present the laboratory which is being used for all of group A 6, most of B 2a, B 3a and B 3 e, and all of B 3b, are: The Laboratory of the Government Chemist (LGC) Queens Road Teddington Middlesex TW11 0LY This laboratory is contracted to collect samples for residue testing by the Veterinary Medicines Directorate, and is responsible in the UK for testing, amongst other things, farmed fish that is destined for human consumption. 3. The laboratory used for the examination of PCB and Dioxin, (B 3a) is: ERGO Forschungsgesellschaft mbH Geierstrasse 1 22305 Hamburg The Laboratory has a quality control, see attachment 3. 4. Mirex, Toxaphene and Chlordane, has been examined at the Institut national de santé puplique QUÉBEC, centre de toxicologie 945 avenue Wolfe Sainte-Foy, Québec Canada G1V 5B3 Method E-448-A, is used. 5. Cantaxanthin (B 3e), has been examined at the Norwegian laboratory: "NIFES Nationalt Institutt for Ernærings- og Sjømatforskning"(NIFES) Postboks 176 Centrum 5804 Bergen Norway 6, Stilbenes and Steroids (A 1) and (A 3), has been examined at the Norwegian laboratory: "Aker universitetssygehus HF" (AS) 2. List of Official Laboratories Trondheimsveien 235 0514 Oslo Norway 7, Mycotoxins (B 3 d), has been examined at the Norwegian laboratory: "Veterinærinstiututtet", Oslo (VIO) Ulleålsveien 68 Pb 8156 Dep. 0033 Oslo Norway
These laboratories are responsible in Norway for testing, amongst other things, farmed fish that is
destined for human consumption.
2.1 Level of Competence of the National Reference Laboratory
Level of Competence of the National Reference Laboratory, as well as Routine Laboratories,
Particularly as Regards to the Implementation of Quality Assurance, or GLP´s (Dec 98/179/EC)
(FVEA) A copy of the Accreditation Certificate for the National Food-, Veterinary- and
Environmental Agency (FVEA), Reference Laboratory, DANAK Accreditation No: 303 is
enclosed. See Attachment 4. Moreover see the webside: www.danak.dk
(LGC)'s laboratory is contracted to collect samples for residue testing by the Veterinary Medicines
Directorate, who is responsible in the UK for the testing of, amongst other things, farmed fish that is
destined for human consumption. Quality controls and standards are run with each batch to ensure
validity of results.
(ERGO) have been working in the field of PCDD/PCDF-analysis since world wide special analyses
began. They have collaborated with national and international partners in industry, authorities (e.g.
Federal Health Office, Germany; Environmental Protection Agency (EPA), USA), universities and
organizations. Their institute has several accreditations and authorization, e.g. the WHO-
authorization (organisation mondiale de la santé, O.M.S.) for the analysis of PCDDs/PCDFs in
human blood and cow's milk. see attachment 3.
(CDT) Institut national de santé puplique QUÉBEC, centre de toxicologie. Moreover see the
(NIFES), "Nationalt Institutt for ernærings-og Sjømatforskning". Their institute has several
accreditations and authorization.
(AS),"Aker universitetssykehus HF". The examination has followed the fundamental principles in
their accreditation. The laboratory is contracted to collect samples for residue testing of group A1
(VIO), Veterinærinstituttet,Oslo. Is accredited according accredited document TEST 110. The
laboratory meets the demands in NS-EN ISO/IEC 17025.
2.2 Details of Analysis Methods - Screening /Routine and Confirmation, with Action Levels
and Detection Limits
Article 7, point 5, pursuant to Council Directive 96/23/EC. 2. List of Official Laboratories 2.2.1 Screening of Stilbenes and Steroides in Fish The diethylstilbestrol assay is intended for qualitative estimation of diethylstilbestrol (DES), hexestrol (HEX), dienestrol (DIEN) and nortestosterone in urine, bile, feed, liver and fish. Fish samples are hydrolysed by enzyme, extracted, defatted and extracted. Hydrolysed substances are clean up with liquid extraction and solid phase extraction before derivatising and terminal points measuring with gas chromatography and mass spectrometry detection (GC-MS) 2.2.2 Confirmation of Stilbenes and Steroides in Fish In addition the confirmation process includes clean up on HPLC, before derivatising and analysing on GC-MS. 2.2.3 Screening test for the detection of Chloramphenicol in Fish muscle by ELISA Fish muscle is homogenised in ethyl acetate. After solvent change to iso-octane/chlorobutane, chloramphenicol is back-extracted into buffer and analysed by ELISA. 2.2.4 B 1 Antibacterial substances The analysis method used is method 6-G-001. The method is a bioassay and was developed at the Norwegian Directorate for Fisheries. Liver tissue is used for the assay. When residues of antibacterial substances are present in the animal, liver tissues usually contain higher concentration of the residue than muscle tissues. In special cases, muscle tissue can also be used. A piece of liver sample is placed on an agar medium containing a sensitive strain of bacteria. If present, antibacterial substances in the tissue will diffuse out into the medium and during the subsequent incubation the growth of the bacteria will be inhibited in a zone around the tissue. The strains of bacteria are: • E. coli to detect qiunolones (oxolinic acid, flumequine). pH in the medium is 7,2. Detection limit is 200 ng/g (µg/kg) • Bacillus cereus to detect tetracyclines and florfenicol. pH in the medium is 5,85. Detection limit is 200 ng/g (µg/kg) • Micrococcus luteus to detect sulfonamides. pH in the medium is 7,3. When residues are detected the sample is sent to the Fødevareregion Ringsted in Denmark for verification and identification. This is done with HPLC. 2.2.5 Screening for Ivermectin ans Emamectin in Salmon by LC/FLUORESCENCE The samples are extracted using anhydrous sodium sulphate and acetonitrile. Extracts are cleaned up by alumina chromatography followed by solid phase (SPE) using C18 cartridges. Residues of samples are derivatised with N-methylimidazole and trifluoroacetic anhydride and then analysed by liquid chromatography (HPLC) with fluorescence detector. Quqlity control and standards are run with each batch to ensure validity of results. 2.2.6 Determination of PCBs, Organochlorine and Pyrethorid pestiside residues in fish The pesticide is extracted from the sample matrix (10g) by blending the test portion with a solvent mixture of (300ml) acetone and hexane. 2. List of Official Laboratories The extract is then collected into a suitable vessel and reduced in volume by evaporation with
nitrogen. A portion of the extract is cleaned up using Gel Permeation Chromatography and Silica
Solid Phase Extraction. An internal standard is then added to the sample extract. Pesticide residues
are then determined in the sample extract by gas chromatography using mass spectrometry
detection and quantification.
The method is suitable for the determination of organochlorine, organ phosphorous, carbamate and
pyrethroid pesticide residues in fish. The limits of quantification for fish are: Organohlorine
pesticide residues: 10µg/kg.
2.2.7 Analytical methods for Organochloriniated pesticides and toxaphenénes congeners.
2.2.8 Analytical methods for PCDD's/PCDF's
The measurements are done by high resolutions mass spectrometry (HRMS), which guarantees high
specificity and high sensitivity.
Before the extraction the following 13C-UL-labeled internal standards are added to the sample:
Table 1. Internal Standards (13C-UL), PCDDs/PCDFs
Internal standards (13C-UL), 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 -Penta-CDF 2,3,4,7,8 -Penta-CDF 1,2,3,4,7,8 -Hexa-CDD 1,2,3,4,7,8 -Hexa-CDF 1,2,3,6,7,8 -Hexa-CDD 1,2,3,6,7,8 -Hexa-CDF 1,2,3,7,8,9 -Hexa-CDD 1,2,3,7,8,9 -Hexa-CDF 2,3,4,6,7,8 -Hexa-CDF 1,2,3,4,6,7,8 -Hepta-CDD 1,2,3,4,6,7,8 -Hepta-CDF 1,2,3,4,7,8,9 -Hepta-CDF 1,2,3,4,6,7,8,9 -Octa-CDD 1,2,3,4,6,7,8,9 -Octa-CDF
After spiking, the samples are extracted with appropriate solvents for ultratrace-analysis (e.g.
nanograde). The clean up is done on multicolumn system involving carbon-on-fibreglass or carbon-
on-celite. The measurement is done by means of high resolution gaschromatgraphy and high
resolution mass spectrometry (HRGC/HRMS) with VG-AutoSpec and/or Finnigan MAT 95 XL
using DB-5 capillary columns. For each substance 2 isotope masses are measured. The
quantification is carried out with the use of internal and external standards.
Table 2. The following PCDDs/PCDFs are reported
2,3,7,8 -Tetra-CDD 2,3,7,8 -Tetra-CDF 1,2,3,7,8 -Penta-CDD 1,2,3,7,8 -Penta-CDF 2,3,4,7,8 -Penta-CDF 1,2,3,4,7,8 -Hexa-CDD 1,2,3,4,7,8 -Hexa-CDF 1,2,3,6,7,8 -Hexa-CDD 1,2,3,6,7,8 -Hexa-CDF 1,2,3,7,8,9 -Hexa-CDD 1,2,3,7,8,9 -Hexa-CDF 2,3,4,6,7,8 -Hexa-CDF 1,2,3,4,6,7,8 -Hepta-CDD 1,2,3,4,6,7,8 -Hepta-CDF 1,2,3,4,7,8,9 -Hepta-CDF 1,2,3,4,6,7,8,9 -Octa-CDD 1,2,3,4,6,7,8,9 -Octa-CDF 2. List of Official Laboratories In addition to the single results, calculations of the toxicity equivalents (TEQ) according to the
WHO-system are carried out.
The measurements are done by high resolution mass spectrometry (HRMS), which guarantees high
specificity and high sensitivity.
Prior the extraction following 13C-UL-labeled internal standards
are added to the sample:
Table 3. Internal standards (13C-UL), WHO-PCBs
Internal standards (13C-UL), WHO-PCBs
3,3´,4,4´ -Tetra-CB 3,4,4´,5 -Tetra-CB 3,3´,4,4´,5 -Penta-CB 3,3´,4,4´,5,5´ -Hexa-CB 2,3,3´,4,4´ -Penta-CB 2,3,4,4´,5 -Penta-CB 2,3´,4,4´,5 -Penta-CB 2´,3,4,4´,5 -Penta-CB 2,3,3´,4,4´,5 -Hexa-CB 2,3,3´,4,4´,5´ -Hexa-CB 2,3´,4,4´,5,5´ -Hexa-CB 2,3,3´,4,4´,5,5´ -Hepta-CB After spiking, the samples are extracted/solved with appropriate solvents for ultratrace-analyses
(e.g. nanograde) by using a solid / lipid extraction.
The clean up is done on multicolumn system (involving carbon-on-fibreglass. The measurement is
done by means of high resolution gaschromatgraphy and high resolution mass spectrometry
(HRGC/HRMS) with VG-AutoSpec and/or Finnigan MAT 95 XL using DB-5 capillary columns.
For each component 2 isotope masses are measured. The quantification is carried out by the use of
internal / external standard mixtures (isotope dilution method). Following PCBs are determined and
Table 4. WHO-PCBs
3,3´,4,4´ -Tetra-CB 3,4,4´,5 -Tetra-CB 3,3´,4,4´,5 -Penta-CB 3,3´,4,4´,5,5´ -Hexa-CB 2,3,3´,4,4´ -Penta-CB 2,3,4,4´,5 -Penta-CB 2,3´,4,4´,5 -Penta-CB 2´,3,4,4´,5 -Penta-CB 2,3,3´,4,4´,5 -Hexa-CB 2,3,3´,4,4´,5´ -Hexa-CB 2,3´,4,4´,5,5´ -Hexa-CB 2,3,3´,4,4´,5,5´ -Hepta-CB In addition to the single results, calculations of the toxicity equivalents (TEQ) according to the WHO-system are carried out. 2. List of Official Laboratories 2.2.10 Marker-PCBs Within the scope of the investigation, the PCBs 28, 52,101,118,138,153 and 180 are determined. Before the extraction the following 13C-UL-labeled internal standards are added to the sample: 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) 2,2´,3,4,4´,5,5´-Hepta-PCB (PCB-180) After the spiking, the samples are extracted with appropriate solvents for ultratraceanalyses (e.g. nanograde). In the following, a column clean up is performed. The measurement is done by means of high resolutions gaschromatography and mass spectrometry (HRGC/MS) using DB-5 capillary columns. For each substance 2 isotope masses are measured. The quantification is carried out with the use of internal/external standard mixtures. 2.2.11 Methods used in determining Pb, Cd and Hg in salmon Methods used in determining Pb, Cd in salmon The analysis is carried out by destruction with nitric acid according to mod. ISO 15587-2, 1.ed., and measurement by atomic absorption in a graphite oven, Analyst 600 according to mod. ISO 11047, 1. ed. At least one reference material is used with each destruction. The samples are determined with reference to a separate calibration curve, but a check is made that the slant is within 85 - 115% of the slant on a curve in which allowance is made for matrix effect. Reference materials The following reference materials are used: Dorm-2, NCR-Canada (shark muscle) BCR No 185, (Bovine liver) Dolt-3, NCR-Canada (shark liver) The values were within our acceptance limits. The detection limits: are 2 µg/kg for Cd and 20 µg/kg for Pb. The uncertainty. is expressed by the maximum relative standard deviation (RSD) on the results from analysing the reference materials. RSD for Cd = 15% and RSD for Pb = 15%. Methods used in determining Hg in salmon The analysis is carried out by destruction in a Berghoff bomber with nitric acid and sulphuric acid and measurement with FIMS 400 (Flow Injection Mercury System) in accordance with Atomic Spectroscopy 1994 15/4 161 -164. At least two results are taken for all samples. At least one reference material is used with each destruction. 2. List of Official Laboratories Reference materials
Dorm 2, NCR, Canada (shark muscle)
Dolt-3, NCR, Canada (shark liver)
The values were within our acceptance limits.
The detection limits are 10 µg/kg for Hg
The uncertainty: is expressed by the maximum relative standard deviation = 20 % on the results
from analysing the reference materials.
We have taken part in the inter calibration "Quasimeme (round 40, exercise 651)", in which Cd, Pb
and Hg were parameters. The results were good.
2.2.12 Malachite Green
About 5g of muscle are weighed to the nearest 0.01g. The sample is then extracted using an
ammonium acetate buffer, dichloromethane and acetonitrile. After centrifugation of the extract and
a liquid-liquid partition, the extract is finally cleaned up on alumina and PRS cartridges. The
subsequent determination of malachite green and leucomalachite green is achieved using LC/MS-
Limit of Detection
The limit of detection is calculated as three times the standard deviation of at least 20 blank
analyses at the appropriate retention time.
Table 5. Limit of Detection
Normal reporting limit for Malachite green is 0.5 µg/kg
And for Leucomalachite green is 1.0 µg/kg
Fat-faction extracted with warm water/acetone and ether. The fraction is cleaning up with water and
the ether phase will be isolated. The solvent is watered and the sample is dissolved in heptan. The
blend will be analysed by normal phase HPLC and detected spectrophotometrically at about 470
nm. *(Methode 044)
2.2.14 Screening and Confirmation of Mycotoxin
The aflatoxins are extracted from a grinded sample with acetonitrile-water (60+40, v/v) for one
hour. The extract is then filtered and diluted with PBS-buffer. A 50 ml portion of this diluted extract
is transferred to an immunoaffinity column. The aflatoxins are then eluted from the column with
totally 1.25 ml of pure methanol and finally diluted with 1,75 ml distilled water.
The aflatoxins is analysed on a reversed phase HPLC system with fluorescents detector and a Kobra
Aflaprep: Application of immunoaffinity columns for sample clean up prior to HPLC or TLC analysis for aflatoxins. RHONE-POULENC DIAGNOSTICS LTD. 2. List of Official Laboratories Methods of Analysis (1990) 15th Ed. AOAC, Arlington, VA, USA, secs 970.44A and 971.22B Detection of Aflatoksin with HPLC after clean up of extract with immunoaffinitetscolumn. Statens Lantbrukskemiska Laboratorium (SSL) method no. 41. Elke Anklam (coordinator) Method for the determination of aflatoxin BG in figs, pistachios, peanut butter and paprika powder. Validated method in the SMT project CT96-2045 for validation of analytical methods for Mycotoxins (1997-1998).
Detection Limit is 0,1 µg/kg
3. National Tolerances for Substances National Tolerances for Substances
3.1 Description of Measures Taken by Competent Authorities When Residues Are Detected
Article 7, point 7-8, pursuant to Council Directive 96/23/EC. We have not detected any medicines in any samples of stock farm fish. No changes have occurred in allowable withdrawal times before harvest. Should a sample test be positive, this would be taken quite seriously. Necessary corrective steps would be taken immediately to protect the consumer. The affected stock farm would be forbidden to sell fish. These food products would be designated unfit for human consumption, pursuant to § 11 of the Food Act, which states: It is not allowed to sell food for general use if it is suspected it will cause illness or poisoning, or if the food, due to pathological changes, putrefaction, pollution, incorrect preparation or by other means can [be] judged unfit for human consumption. 3.1.1 Category A Substances: All fish from the sampled population will be declared unfit for human consumption and destroyed. (However, it may be necessary and prudent to conduct further testing to verify the initial test results.) 3.1.2 Category B1 Substances: If the fish are alive, they will be held for the requisite withdrawal time before harvest pursuant to regulations in force, and until no detectable residues of the medicines remain. If the fish from the sampled population have already been harvested, they will be declared unfit for human consumption and destroyed. The stock farms that produced the affected fish will be properly and thoroughly tested to determine the exact reasons for the positive result, prior to being granted permission to use medicines. Suitable arrangements will be made with the stock farm in order to ensure against repeat occurrences. 4. Scope of the Residue Plan Scope of the Residue Plan
4.1 Group of Residues Covered
Group of Residues Covered (as listed in Annex I). Breakdown of Substances Monitored in Each Group by Animal Species and Product (Table). Article 7, point 5, pursuant to Council Directive 96/23/EC. 4.1.1 The following changes have been made from the previous report: The survey of used medicines in 2004, from the Chief Pharmaceutical Officer was not carried out before September 2005, due to problems with the computer data. The survey of used medicines in 2004 and 2005 is stated in this report (see attachment 8) 4.1.2 The category A, substances: The likelihood to detect Stilbenes, Steroides or Chloramphenicol in salmon or trout, from aquacultur is very low. Therefor, and also based on previous experience and data from from the Chief Pharmaceutical Officer, we do have decided to pool 5 or 6 samples in each analysis. 4.1.3 Sulfonamides The inhibition zone against the sulfadimidiene sensitab is smaller than usual. The sulfonamid tesults has to be taken with some reservations, but referring to data from the Chief Pharmaceutical Officer, attachment 8, we dont have used any sulfonamid the last three years. Results 2005
Table 6. Results 2005, Group A
Group of substances Tissue to be Laboratory Detection Level of No. Of Diethylstilboestrol Stilbenes/Dienestrol Hexestrol/Dienestrol Chloramphenicol Muscle ELISA 0,3µg/kg (An.IV of CR 2377/90) Total number of samples in Group A: 121
4. Scope of the Residue Plan
Table 7. Results 2005, Group B
Group of substances Compounds Tissue to be Laboratory Detection Level No. Of B 1 Antibacterial Quinolones (oxolinacid, Liver G-038 200ppb Tetracycline, florfenicol Liver Liver G-038 400ppb B 2 a Anthelmintics Ivermectin Muscle Emamectin Muscle LC/MS-MS 50µg/kg Deltametrin Muscle Cypermethrine Muscle B 3 a Organoclorine pp-DDE HCH incl. Lindane DDT's pp-TDE Mirex Toxaphene (Nonachlor) Dichlorvos Muscle Organophosphorus Azametiphos Muscle Chemical Elements <20 µg/kg 300 <2 µg/kg 500 B 3 d Mycotoxins Fluorescence µg/kg Feeding HPLC 0,2 LC/MS-MS 2 µg/kg Total number of samples in Group B: Total number of samples in # Including, pp-DDT, op-DDT, pp-DDE, pp-TDE, HCB, A-HCH, G-HCH, B-HCH. * Including PCB 28, PCB 52, PCB 101, PCB 138, PCB 153, PCB 180, PCB 118 4. Scope of the Residue Plan
¤ Including alpha/gamma and oxy-chlordane. Cis/trans-nonachlor
Malachite Green includes leuco-machite green
The results are detailed in attachment 5.
The samples are divided among these stock farms, see attachment 6.
5. Residues Plan for the Examination in Aquaculture Products 2006 Residues Plan for the Examination in Aquaculture Products
The annual plan for the examination for residues in aquaculture products in the Faroe Island, for the
Table 8. Annual plan for the examination for residues, Group A
Group of substances Compounds Laboratory Detection Level of action No. Of be analysed method Samples analysed Diethyl-stilboestrol Muscle Chloram-phenicol Muscle ELISA 1µg/kg Pos. Detection 30 L samples in group A 5. Residues Plan for the Examination in Aquaculture Products 2006
Table 9. Annual plan for the examination for residues, Group B, and Totals
Group of substances Compounds Tissue to be Laboratory Detection Level of action No. Of Samples analysed B 1 Antibacterial Liver G-038 200ppb (oxolinacid, flumequine Tetracycline, Liver G-038 200ppb Pos. Detection 60 florfenicol Sulfonamides Liver G-038 400ppb B 2 a Anthelmintics Ivermectin Muscle LC/MS-MS Emamectin Muscle LC/MS-MS Deltametrin Muscle GCMS 50µg/kg Cypermethrine Muscle Chlordane Muscle GC/EDC Toxaphene Muscle Marker-PCBs Muscle HRGC/MS WHO-PCBs Muscle HRGC/MS Dichlorvos Muscle GCMS 10µg/kg Azamethiphos Muscle AAS,grafit, <20µ/kg AAS,grafit, <2µg/kg 50 FIMS/AMA <2µg/kg 500 B 3 d Mycotoxins Malachite green Muscle LC/MS-MS 2 µg/kg Cantacantin Feeding Total number of samples in group B: Total number of samples in Group A + Group B: This is a preliminary plan, and based on our experience in getting laboratories involved. It may well be that the residue plan for 2006 will be revised. 6. Background Information on Production Background Information on Production
6.1 Animal Species and Total Figures of Production
6.1.1 Animal Species
6.1.2 Production Totals
Aquaculture product exports (kilograms) from the Faroe Islands. (See Table 10.)
Table 10. Exports in Aquaculture Products from the Faroe Islands
2002 2003 2004 2005 Exports in Aquaculture Products, Total kg's. 43.399.252 47.644.000 34.818.000 18.365.000 From the Faroe Islands
6.2 Type of Production
Type of Production of 2.1 (Intensive, Extensive, Wild or mixed Systems) (Annex IV)
Type of Production: All production is INTENSIVE production.
Every fish is processed in approved facilities, according to EU Directive 91/493.
See Attachment 2. A list of approved factories, which export to the EU.
7. Frequencies and Levels of the Controls Frequencies and Levels of the Controls
7.1 Number of samples
Number of samples to be taken for each sub-group of substances in the case of each species/product by reference to the number of animals slaughtered and volume of product output of animal origin in the previous year (Annex IV and Dec 97/ 747/EC). See check table, (Attachment 7). In 2005 the export of salmon and trout was Of this the export to the EU was
This means that in 2006 altogether 184 samples should be taken for testing for residues of
medicines. Section 5 and 6. The residue plan in section 5 may be revised.
The table for checking is provided in accompanying Attachment 7.
8. Targeting Criteria Targeting Criteria
All tests which we have done so far have been under the tolerance limits. They were all conducted
according to the methodology described in Section 2.3.
The residue plan for 2006 has been based on the plan for 2005, and partly according to which
medicines are, and have been, used in the Faroese in recent years, see attchment 8.
8.1 Changes Based on Analyses of the Residue Plan of the Previous Years
Changes Based on Analyses of the Residue Plan of the Previous Years (Where Such Plans Exist)
Particularly as Regards Problem Areas Identified.
Refer to Article 8, point 2, pursuant to Council Directive 96/23/EC.
The Agency has not identified any problems in the problem areas referred to.
The Agency drafted a plan for 2005 to respond to the requirements in Annex I, II, III and Annex IV
(Chapter 3) in Council Directive 96/23/EC. See Section 7.
Tórshavn, 30th March 2006
Faroese Food-, Veterinary and Environmental Agency
Óluva Niclasen, Head of Department
OLFAR: ADAPTIVE TOPOLOGY FOR SATELLITE SWARMS A. Budianu University of Twente, Faculty of Electrical Engineering, Mathematics and Computer Science, Telecommunication Engineering Group, P.O. Box 217, 7500 AE, Enschede, The Netherlands R. T. Rajan1, S. Engelen2, A. Meijerink3, C. J. M. Verhoeven2 and M. J. Bentum4 Abstract—Low-frequency space observation is one of the de-