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Published on behalf of
Commission of the European Communities
Residues in food producing
animals and their products:
Reference Materials and Methods
Second Edition
Edited by R.J.Heitzman
Directorate REPORT Measurements and
General Eur15127-EN Testing (BCR)
for Agriculture Directorate General
EC Brussels Science, Research and
EC Brussels
Published on behalf of
Commission of the European Communities
Residues in food producing animals and their products:
Reference Materials and Methods.
Second Edition
Edited by
1, Chum Road
Berkshire RG16 OPP
United Kingdom
Contract Numbers 5464/1/5/272/91/04-BCR-UK(10) & 5326/1/5/272/90/3-BCR-UK(10)
Final Report
Measurements and Testing Programme (BCR)
Directorate General for Science, Research and Development
Directorate for Agriculture.
PARI fUROP, Biblioth.
Sg 4.1. Tranquillizers - An HPLC method with on-line UV spectrum
identification by diode-array for residues in pig kidneys.
[Origin, The Netherlands]
Sg 4.2. Carbadox as QCA - routine screening method for the
determination by HPLC of quinoxaline carboxylic acid (QCA) in
pig kidney tissue. [Origin, UK]
Sg 4.3 Carbadox as Desoxycarbadox - routine screening method for the
determination by HPLC of Carbadox and Desoxycarbadox in pig
meat, liver and kidney tissue. [Origin, The Netherlands]
Sg 4.4 Ionophores - a routine method for the determination of residues
of ionophores in chicken meat, liver and kidney using HPTLC.
[Origin, The Netherlands]
Sg 4.5 Levamisole - a routine method for then of residues
of levamisole in liver tissue by GC-MS. [Origin, UK]
Cy 1.1. Anabolic Agents - A modular method for the analysis of
biological materials for residues of anabolic agents. [Origin;
The Netherlands and Italy]
Cy 1.2. Anabolic Agents - A multi-residue method for determining
residues of anabolic agents in animal tissues. [Origin;
1.3. Stilbenes - Confirmation of stilbenes in bile by gas Cy
chromatography-mass spectrometry. [Origin; UK]
1.4. Trenbolone -n of trenbolone in bile by gas Cy s spectrometry [Origin;
1.5. Zeranol - Confirmation of zeranol in bile by gas Cy s spectrometry. [Origin; UK]
1.6* Zeranol - Method for measurement of residues of zeranol in Cy
animals and animal tissues using HPLC/radioimmunoassay (RIA).
[Origin; The Netherlands and UK]
1.7* Stilbenes - Method for the measurement of residues of the Cy
stilbenes, diethylstilboestrol, hexoestrol and dienoestrol in
animals and animal tissues on the basis of HPLC/RIA. [Origin;
The Netherlands and UK]
1.8. Ethinyloestradiol - Method for the measurement of residues of Cy
ethinyloestradiol in cattle urine by GC-MS [Origin; Belgium]
1.9. Thyreostats - method for the measurement of residues of Cy
thyreostatic substances in animals and animal tissues on the
basis of high performance thin layer chromatography and gas
chromatography - mass spectrometry (GC-MS). [Origin, Belgium]
Cy 2.1 B-agonists - a method for the detection and identification of
B-agonists in biological samples and animal feed.[Origin; The
Cy 2.2. Clenbuterol - Determination of clenbuterol at residue levels in
bovine plasma and tissues by GC-MS. [Origin; France]
Cy 2.3. B-Agonists - a method for confirming the detection of B-
agonists in bovine urine by GC-MS in the positive chemical
ionisation mode for the trimethylsilyl derivatives. [Origin,
[Note; The use of spectroscopic methods for the confirmation of the
stilbenes and zeranol is preferred]. Cy 3.0 METHODS FOR ANTIBIOTICS
Cy 3.1. Sulphonamides - Confirmation of sulphonamides by GC-MS.
[Origin; UK]
Cy 3.2 Sulphadimidine. Determination of sulphadimidine in pig kidney
and diaphragm muscle tissue by high performance liquid
chromatography. [Origin UK-NI]
Sulphadimidine - HPLC analysis ofe in porcine Cy 3.3
kidney. [Origin; UK]
3.4 Sulphadimidine. Determination of sulphadimidine in reference cy
material and fresh tissues by high performance liquid
chromatography. [Origin UK-NI]
3.5 Chloramphenicol - Confirmation of chloramphenicol in meat, cy
eggs, milk and urine by GC-MS. [Origin; The Netherlands]
3.6 l -n ofl in meat by Cy
GC-MS [Origin; Germany]
3.7 Chloramphenicol - HPLC analysis of chloramphenicol in milk. cy
[Origin; France]
3.8 Tetracyclines - Determination by HPLC of tetracyclines at Cy
residue levels in animal tissues. [Origin; UK]
3.9 Nitrofurans - HPLC combined with dialysis for determining Cy
residues of nitrofurans in eggs, milk and meat. [Origin; The
Benzimidazoles - Determination by HPLC of Benzimidazole type 4.1
anthelmintics at residue levels in animal tissues and milk.
[Origin; UK]
4.2 Lasalocid - Determination by HPLC of Lasalocid at residue Cy
levels in poultry muscle and eggs. [Origin; UK]
Carbadox -n by GC-MS of quinoxaline carboxylic 4.3 cy
acid (QCA) at residue levels in kidney tissue. [Origin; UK]
Ivermectin - Determination by HPLC of Ivermectin at residue 4.4 Cy
levels in animal tissues.[Origin; UK]
4.5 Tranquillizers and carazolol - an HPLC method with on-line UV cy
spectrum identification and off-line TLC confirmation for
residues in pig kidneys. [Origin; The Netherlands]
Cy 4.6. Tranquillizers - Identification using GC-MSn for
residues of tranquillizers in pig kidneys. [Origin; The
Netherlands] 1. INTRODUCTION
The Council Directive (86/469/EEC) concerning the examination of animals
and fresh meat for the presence of residues requires that samples are
analyzed "in accordance with methods which are applied by Member States and
have been submitted to the Commission under their inspection plans". These
methods are routine methods of analysis for screening and confirmation
purposes. All positive findings must, if challenged, be confirmed by a
laboratory officially approved for that purpose by the competent
authorities, using the reference methods established pursuant to Article
4(l)(b) of Directive 64/433/EEC.
This manual brings together those parts of EEC legislation concerned with
residues, the National Surveillance programmes for residues, and the latest
progress and developments in routine methods and Reference Materials (RMs).
More specifically the purpose of the manual is to provide a reference
manual describing the methods and materials (standards ande
materials) for use in the identification, measurement and confirmation of
residues in food of animal origin.
Analytical technology is continually changing and progressing. Thus in the
first edition in 1991 methods were reported at various advanced stages of
development and with special emphasis on multi-residue and modular methods.
In this edition there are more methods, including a new section describing
a selection of routine screening methods used by Member States. The
routine methods used throughout the Community are summarised in table form
for each analyte. Where possible the routine methods are differentiated as
screening or confirmatory methods.
For many analytes there are excellent confirmatory methods used by one or
more Member States which for a variety of reasons have not yet been raised
to the status of Reference Methods. Until such time as a reference method
is available a selection of these routine confirming methods is detailed.
Many of these methods are probable candidates for Reference Methods.
This edition includes a section on quality assurance which complements the
criteria for methods set out in EEC Decision 93/256 and reproduced in
section 5.
The book is aimed primarily for use in reference laboratories or other
laboratories performing residue analysis. Many international and national
authorities may also find the book helpful as a reference work for problems
associated with residues.
The routine confirming methods as defined in EEC 93/256 and used by Member
States may in the future be approved by the Commission and given the status
of Community Reference Methods. Reference methods could be used to settle
disputes (e.g between Member States) by providing an approved analytical
tool for the means of controlling residues in food through the specific and
accurate determination of the residue content in food. The routine
confirming methods when fully developed meet the criteria in EEC 93/256
(see section 5) and are suitable for
(i) being performed in EEC reference laboratories,
(ii) identifying unambiguously an analyte (residue)
(iii) measuring the concentration of analytes accurately.
The purpose of the RMs is the quality control of analytical methods by;-
(i) use in development of a method
(ii) determination of accuracy and precision
(iii) quality assurance
(iv) providing RMs with concentrations of analytes at or near the
tolerance limits (MRL) set by the EEC or when MRL are zero at or
close to the lower limit of detection of the method.
(v) a standard for traceability
The RMs will be available commercially through the Measurement and Testing
Programme of DG12. Certified RMs are now available for the stilbenes in
bovine urine.
RMs are stable materials of animal origin containing residues at known
concentrations. They are prepared by collecting samples (muscle, liver,
kidney, fat, bile, urine, blood or faeces) from animals administered
veterinary drugs or other substances. The samples are prepared as
lyophilised material which are stable and have stated residue

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