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European legislation on methods for antibiotics detection in milk (Council Regulation 2377/90/EC, Council Directive 96/23/EC and Commission Decision 2002/657/EC)

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Presentation on theme: "European legislation on methods for antibiotics detection in milk (Council Regulation 2377/90/EC, Council Directive 96/23/EC and Commission Decision 2002/657/EC)"— Presentation transcript:

1 European legislation on methods for antibiotics detection in milk (Council Regulation 2377/90/EC, Council Directive 96/23/EC and Commission Decision 2002/657/EC) Marie-Louise Scippo University of Liège – Laboratory of Food Analysis Belgium mlscippo@ulg.ac.be http://www.adaoa.ulg.ac.be/

2 ML Scippo - Belgrade - 25 September 2008 2  Aminoglycosides and aminocyclitols: (streptomycine, spectinomycine, …)   -lactamins: (penicillins et cephalosporins)  Macrolides: (erythromycine, …)  Peptides (avoparcine, …)  Sulfonamides (sulfamethazine, …)  Trimetroprim  Tetracyclines: (oxy- and chlortetracycline, …)  Phenicols: (chloramphenicol, …)  ionophores (monensine, …)  nitrofurans (furazolidone,…)  quinolones and fluoroquinolones Main « chemical » classes of antimicrobials

3 ML Scippo - Belgrade - 25 September 2008 3  Aminoglycosides and aminocyclitols: (streptomycin, spectinomycin, …)   -lactamins: (penicillins and cephalosporins)  Macrolides: (erythromycin, …)  Peptides (bacitracin, …)  Sulfonamides (sulfamethazin, …)  Trimetroprim  Tetracyclines: (oxy- and chlortetracycline, …)  Phenicols: (chloramphenicol, thiamphenicol )  ionophores (monensine, …)  nitrofurans (furazolidone,…)  quinolones and fluoroquinolones Allowed in lactating cows in EU

4 ML Scippo - Belgrade - 25 September 2008 4 European legislation Council Regulation EEC N°2377/90 (MRLs) Council Directive 96/23/EC (Monitoring of Residues) Commission Decision 2002/657/EC (Criteria for Analytical Methods of Determination of Residues) amended by Commission Decision 2003/181/EC (mRPLs for Chloramphenicol) Commission Decision 2005/34/EC (products imported from third countries, mRPLs = MRLs) http://europa.eu.int/eur-lex/lex/RECH_consolidated.do

5 ML Scippo - Belgrade - 25 September 2008 5 European legislation Council Regulation EEC N°2377/90 (MRLs) Council Directive 96/23/EC (Monitoring of Residues) Commission Decision 2002/657/EC (Criteria for Analytical Methods of Determination of Residues) amended by Commission Decision 2003/181/EC (mRPLs for Chloramphenicol) Commission Decision 2005/34/EC (products imported from third countries, mRPLs = MRLs)

6 ML Scippo - Belgrade - 25 September 2008 6 Council Regulation EEC N°2377/90 Four annexes: - Authorized substances (annexes I, II or III) - Forbidden substances (annex IV, substances for which no MRL can be fixed) (ex. chloramphenicol, nitrofurans, …)

7 ML Scippo - Belgrade - 25 September 2008 7 Council Regulation EEC N°2377/90 Four annexes: 2377/90/Annex I: substances for which MRLs have been fixed by EMEA* 2377/90/Annex II: substances not subject to maximum residue limits (generally recognized as safe) 2377/90/Annex III: substances for which provisional MRLs have been fixed 2377/90/Annex IV: substances for which no maximum levels can be fixed 2377/90/Annex V: information and data needed for the establishment of the MRL  (identity of the substance, toxicological research, metabolism, residues)  Substances with insufficiency of data: not authorised to be used for food-producing animals in the EU *EMEA: European Medicines Agency, http://www.emea.europa.eu/home.htm http://www.emea.europa.eu/home.htm

8 ML Scippo - Belgrade - 25 September 2008 8 Council Regulation EEC N°2377/90 140 modifications up to now..........

9 ML Scippo - Belgrade - 25 September 2008 9 Council Regulation EEC N°2377/90 Example (extract from 2377/90/Annex I, list of authorized substances with fixed MRL)

10 ML Scippo - Belgrade - 25 September 2008 10

11 ML Scippo - Belgrade - 25 September 2008 11 MRLs (in bovine milk) of antibiotics from Annex I of Council Regulation 2377/90/EC Examples

12 ML Scippo - Belgrade - 25 September 2008 12 Antibiotic forbidden in food animals According to Annex IV of Council Regulation 2377/90/EC

13 ML Scippo - Belgrade - 25 September 2008 13 European legislation Council Regulation EEC N°2377/90 (MRLs) Council Directive 96/23/EC (Monitoring of Residues) Commission Decision 2002/657/EC (Criteria for Analytical Methods of Determination of Residues) amended by Commission Decision 2003/181/EC (mRPLs for Chloramphenicol) Commission Decision 2005/34/EC (products imported from third countries, mRPLs = MRLs)

14 ML Scippo - Belgrade - 25 September 2008 14 Council Directive 96/23/EC Member states : Monitoring plans for the detection of residues or substances in live animals, their excrements and body fluids, and in tissue, animal products, animal feed and drinking water

15 ML Scippo - Belgrade - 25 September 2008 15 Council Directive 96/23/EC National plan of control according : 96/23/ Annex I : Groups of residues and substances (group A and B) 96/23/ Annex II : residue or substance group by type of sample

16 ML Scippo - Belgrade - 25 September 2008 16 Council Directive 96/23/EC National plan of control according :  96/23/ Annex I : Groups of residues and substances (group A and B) GROUP A Substances having anabolic effect and unauthorized substances GROUP B Veterinary drugs and contaminants  96/23/ Annex II : residue or substance group by type of sample

17 ML Scippo - Belgrade - 25 September 2008 17 Council Directive 96/23/EC 96/23/ Annex I : Groups of residues and substances (group A and B) GROUP A : Substances having anabolic effect and unauthorized substances A1. Stilbenes and derivatives (DES, …) A2. Antithyroid agents (Tapazole, thiouracyle,…) A3. Steroids (estrogens, androgens, gestagens) A4. Resorcylic acide lactones including zeranol A5. b-agonists (clenbutérol, salbutamol,…) A6. Compounds included in Annex IV to Council Regulation N°2377/90 NO MAXIMAL LEVEL

18 ML Scippo - Belgrade - 25 September 2008 18 Council Directive 96/23/EC 96/23/ Annex I : Groups of residues and substances (group A and B) GROUP B : Veterinary drugs and contaminants B1. Antibacterial substances, including sulphonamides, quinolones B2. Other veterinary drugs 2377/90/EC B3.Other susbtances and environmental contaminants other European Regulations on contaminants and pesticides MAXIMAL LEVEL

19 ML Scippo - Belgrade - 25 September 2008 19 Council Directive 96/23/EC 96/23/ Annex I : Groups of residues and substances (group A and B) GROUP B : Veterinary drugs and contaminants B2. Other veterinary drugs a) Anthelmintics b) Anticoccidials, including nitroimidazoles c) Carbamates and pyrethroids d) Sedatives e) Non-steroidal anti-inflammatory drugs (NSAIDs) f) Other pharmacologically active substances MAXIMAL LEVEL

20 ML Scippo - Belgrade - 25 September 2008 20 Council Directive 96/23/EC 96/23/ Annex I : Groups of residues and substances (group A and B) GROUP B : Veterinary drugs and contaminants B3.Other susbtances and environmental contaminants a) Organochlorine compounds including PCBs b) Organophosphorous compounds c) Chemical elements (Pb, Cd, Hg,…) d) Mycotoxins (aflatoxins, ochratoxin,…) e) Dyes f) Others MAXIMAL LEVEL

21 ML Scippo - Belgrade - 25 September 2008 21 Council Directive 96/23/EC 96/23/ Annex II : residue or substance group by type of sample Bovine, ovine, porcine, equine, animals PoultryAquaculture animals MilkEggsRabbit meat and the meat of wild game and farmed game Honey A1XXXX 2XXX 3XXXX 4XXX 5XXX 6XXXXXX

22 ML Scippo - Belgrade - 25 September 2008 22 Council Directive 96/23/EC 96/23/ Annex II : residue or substance group by type of sample Bovine, ovine, porcine, equine, animals PoultryAquaculture animals MilkEggsRabbit meat and the meat of wild game and farmed game Honey B1 XX X X X X X B2 XX X X 3a XX X X X X X bXXX cXXXXXX dXXXX eX

23 ML Scippo - Belgrade - 25 September 2008 23 European legislation Council Regulation EEC N°2377/90 (MRLs) Council Directive 96/23/EC (Monitoring of Residues) Commission Decision 2002/657/EC (Criteria for Analytical Methods of Determination of Residues) amended by Commission Decision 2003/181/EC (mRPLs for Chloramphenicol) Commission Decision 2005/34/EC (products imported from third countries, mRPLs = MRLs)

24 ML Scippo - Belgrade - 25 September 2008 24 Commission Decision 2002/657/EC

25 ML Scippo - Belgrade - 25 September 2008 25 Commission Decision 2002/657/EC Content : - 11 paragraphs - 10 articles - Annex I : Performance criteria of analytical methods - Annex II : minimum required performance limits

26 ML Scippo - Belgrade - 25 September 2008 26 Commission Decision 2002/657/EC – Annex II Commission Decision 2005/34/EC (products imported from third countries, mRPLs = MRLs)

27 ML Scippo - Belgrade - 25 September 2008 27 Commission Decision 2002/657/EC

28 ML Scippo - Belgrade - 25 September 2008 28 Commission Decision 2002/657/EC

29 ML Scippo - Belgrade - 25 September 2008 29 Commission Decision 2002/657/EC

30 ML Scippo - Belgrade - 25 September 2008 30 Commission Decision 2002/657/EC   5 % Substances of group B / Annex I / 96/23/CE

31 ML Scippo - Belgrade - 25 September 2008 31 Commission Decision 2002/657/EC   5 % Substances of group B / Annex I / 96/23/CE

32 ML Scippo - Belgrade - 25 September 2008 32 Commission Decision 2002/657/EC   1 % Substances of group A / Annex I / 96/23/CE

33 ML Scippo - Belgrade - 25 September 2008 33 Commission Decision 2002/657/EC   1 % Substances of group A / Annex I / 96/23/CE

34 ML Scippo - Belgrade - 25 September 2008 34 < LOD ou < LMR > LOD ou > LMR General strategy of residues monitoring < LOD ou < LMR > LOD ou > LMR

35 ML Scippo - Belgrade - 25 September 2008 35 Analytical methods Qualitative method (substances of 96/23/Annex I/Group A) Quantitative methods (substances of 96/23/Annex I/Group B) Screening method (ELISA, rapid tests,...) Detection of residues (absence or suspicion of presence) (semi-quantitative) Confirmatory method (GC or LC-MS) Detection and identification of residues (absence or presence) Detection, identification and quantification

36 ML Scippo - Belgrade - 25 September 2008 36 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 1. DEFINITIONS (accuracy, precision, repeatability,...) 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.1. GENERAL REQUIREMENTS 2.2. SCREENING METHODS 2.3. CONFIRMATORY METHODS FOR ORGANIC RESIDUES AND CONTAMINANTS 2.4. CONFIRMATORY METHODS FOR ELEMENTS 3. VALIDATION

37 ML Scippo - Belgrade - 25 September 2008 37 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.1. GENERAL REQUIREMENTS Sample handling : avoid cross contamination or analyte loss. Recovery : the percentage of the true concentration of a substance recovered during the analytical procedure. Specificity : the ability of a method to distinguish between the analyte being measured and other substances.

38 ML Scippo - Belgrade - 25 September 2008 38 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.2. SCREENING METHODS false negative rate < 5 % (at the level of interest) MRL

39 ML Scippo - Belgrade - 25 September 2008 39 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.3. CONFIRMATORY METHODS shall provide information of the chemical structure of the analyte (suitable combination of clean-up, chromatographic separation and spectrometric detection) - Criteria of performance - system of identification points

40 ML Scippo - Belgrade - 25 September 2008 40 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.3. CONFIRMATORY METHODS shall provide information of the chemical structure of the analyte (suitable combination of clean-up, chromatographic separation and spectrometric detection) - Criteria of performance - system of identification points

41 ML Scippo - Belgrade - 25 September 2008 41

42 ML Scippo - Belgrade - 25 September 2008 42 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.3.1. Common performance criteria and requirements Choice of the method ! Internal standard Reference material Quality control samples (compliant and non compliant) Reagent blanks

43 ML Scippo - Belgrade - 25 September 2008 43 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.3.2. Additional performance criteria and other requirements for quantitative methods of analysis

44 ML Scippo - Belgrade - 25 September 2008 44 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.3.2. Additional performance criteria and other requirements for quantitativ methods of analysis 22 %

45 ML Scippo - Belgrade - 25 September 2008 45 MRL = 4 µg/Kg

46 ML Scippo - Belgrade - 25 September 2008 46 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.3.3. Performance criteria and other requirements for mass spectrometric detection Retention time (RT) : RT of the analyte should match the RT of the calibration standard (tolrance of ± 0.5 % in GC and 2.5 % in LC). Ion intensity.

47 ML Scippo - Belgrade - 25 September 2008 47 Commission Decision 2002/657/EC

48 ML Scippo - Belgrade - 25 September 2008 48 Commission Decision 2002/657/EC Relative Abundance 300 RT:5.29-5.34NL:2.84E7 F: + c APCI Full ms [ 180.00-350.00] 200210220230240250260270280290 m/z 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 277 279 203 259 205 261 281 207 263 275 282209 217249221 244 223298258 287264242252230294 clenbuterol 35 %30 % Max variation of 25% in unknows

49 ML Scippo - Belgrade - 25 September 2008 49 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 2. PERFORMANCE CRITERIA ANDOTHER REQUIREMENTS FOR ANALYTICAL METHODS 2.3.3. Performance criteria and other requirements for mass spectrometric detection Retention time (RT) : RT of the analyte should match the RT of the calibration standard (tolrance of ± 0.5 % in GC and 2.5 % in LC). Ion intensity. Identification points

50 ML Scippo - Belgrade - 25 September 2008 50 Commission Decision 2002/657/EC

51 ML Scippo - Belgrade - 25 September 2008 51 Commission Decision 2002/657/EC Subst of gr A (96/23/CE, Annex I): At least 4 points Subst of gr B : (96/23/CE, Annex I): At last 3 points

52 ML Scippo - Belgrade - 25 September 2008 52 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 3. VALIDATION

53 ML Scippo - Belgrade - 25 September 2008 53 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 3. VALIDATION Specificity (check for interfering compounds) Trueness (CRM, n=6 replicates) Recovery (if no CRM, fortified samples) Stability (of calibration solutions, of analyte in matrix) Repeatability, reproducibility (including within laboratory) Decision limit CC  Detection capability CC  Calibration curve (at least 5 levels, definition of the working range, r 2 ) Ruggedness (minor and major changes

54 ML Scippo - Belgrade - 25 September 2008 54 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 3. VALIDATION Repeatability (n=6) At 3 levels Substances with mRPL : 1, 1.5 and 2 times the mRPL Substances with MRL : 0.5, 1 and 1.5 times the MRL

55 ML Scippo - Belgrade - 25 September 2008 55 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 3. VALIDATION Within laboratory reproducibility (n=6 replicates/serie, 3 independent series ) At 3 levels Substances with mRPL : 1, 1.5 and 2 times the mRPL Substances with MRL : 0.5, 1 and 1.5 times the MRL

56 ML Scippo - Belgrade - 25 September 2008 56 Commission Decision 2002/657/EC 2002/657 Annex I : Performance criteria of analytical methods 3. VALIDATION Reproducibility Participation to collaborative studies according to ISO 5725-2 (Basic method for the determination of repeatability and reproducibility of a standard measurement method).

57 ML Scippo - Belgrade - 25 September 2008 57 Commission Decision 2002/657/EC Decision limit (CC  ): example N = 20 fortified samples at the MRL CC  = MRL + 1.64 

58 ML Scippo - Belgrade - 25 September 2008 58 Commission Decision 2002/657/EC Detection capability (CC  ): example

59 ML Scippo - Belgrade - 25 September 2008 59 Directive 96/23/EC EUROPEAN COMMISSION CVMP NATIONAL PLAN MEMBER STATE Sample Analytes Methods ANALYSES METHODS CRITERIA (DC 2002/657/EC) Other labs NRL CRL CRMs MRLs REPORTS MRLs: Maximum Residue Limits CVMP: Permanent Vet. Med. Commitee NRL: National Reference Laboratories CRL: Community Reference Laboratories CRMs: Certified Reference Materials

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