1. 6.12.2011ÚKZÚZ - NRL RO Praha1 COMMISSION REGULATION (EC) No 152/2009 of 27 January 2009 laying down the methods of sampling and analysis for the official control of feed Ing. Petrová Jaroslava Workshop on Official Controls of Feed AGR 46230, 6. – 7. 12. 2011, Ankara. Turkey

2. 6.12.2011ÚKZÚZ - NRL RO Praha2 Content of „Methods of analysis for the official control of feed „ presentation 1. Legal reasons for analysis food samples for the official control Identification of methods 2. Laboratory requirements 3. History of Methods of analysis for the official control of feed 4. Content of Regulation 152/2009 5. Analytical methods other than methods for official control 6. Requirements on methods validated in one laboratory

3. 6.12.2011ÚKZÚZ - NRL RO Praha3 Regulation 767/2009 - Official control in laboratory (i n the placing on the market and use of feed,) ANNEX I - Chemical impurities from techological process, - botanical impuritues - iron level in milk replacers - denaturants, binders - ash insoluble in HCl - water content Annex V, VI - Crude protein - Crude fibre - Starch - crude fat and oil - crude ash - lysin, methionin - Ca, Na, P, Mg Article 15 - addives

4. 6.12.2011ÚKZÚZ - NRL RO Praha4 Regulation 882/2004 on official controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules Article 12 - Laboratory(ies) for official control are named by competend national authorities - Laboratory(ies) for official control should be accredited (EN ISO/IEC 17025 on ‘General requirements for the competence of testing and calibration laboratories) (ÚKZÚZ is accredited since 1994)

5. 6.12.2011ÚKZÚZ - NRL RO Praha5 Summary - Official control obey the same legislation as production - Analytical laboratories should be accredited and analytical method should be validated - Official analytical method ensure credibility and comparability of laboratory results

6. 6.12.2011ÚKZÚZ - NRL RO Praha6 Methods of analysis for the official control of feed - History 1970 – Directive 70/373/EEC Directives establishing Community methods of analysis for the official control of feedingstuffs: 1971 – First Commission Directive 71/250/EEC of 15 June 1971. Second Commission Directive 71/393/EEC of 18 November 1971 Third Commission Directive 72/199/EEC of 27 April 1971 1972 - Fourth Commission Directive 73/46/EEC of 5 December 1972 1976 - Seventh Commission Directive 76/372/EEC of 1 March 1976 1978- Eight Commission Directive 78/633/EEC of 15 June 1978 1981 - Ninth Commission Directive 81/715/EEC of 31 July 1981 1984 - Tenth Commission Directive 84/425/EEC of 25 July 1984 1993 - Eleventh Commission Directive 93/70/EEC of 28 July 1993 2003 - Commission Directive 2003/126/EC of 23 December 2003 on the analytical method for the determination of constituents of animal origin for the official control of feedingstuffs ….2009 2009- COMMISSION REGULATION (EC) No 152/2009 of 27 January 2009 laying down the methods of sampling and analysis for the official control of feed

7. 6.12.2011ÚKZÚZ - NRL RO Praha7 Regulation 152/2009 methods of analysis ANNEX II GENERAL PROVISIONS ON METHODS OF ANALYSIS FOR FEED C. APPLICATION OF METHODS OF ANALYSIS AND EXPRESSION OF THE RESULTS 1. Extraction procedure Several methods determine a specific extraction procedure. As a general rule, other extraction procedures than the procedure referred to in the method can be applied on the condition that the used extraction procedure has been proven to have the equivalent extraction efficiency for the matrix analysed as the procedure mentioned in the method 2. Clean-up procedure Several methods determine a specific clean-up procedure. As a general rule, other clean-up procedures than the procedure referred to in the method can be applied on the condition that the used clean-up procedure has been proven to result in equivalent analytical results for the matrix analysed as the procedure mentioned in the method

8. 6.12.2011ÚKZÚZ - NRL RO Praha8 Regulation 152/2009 methods of analysis A. Determination of moisture B. Determination of moisture in animal and vegetable fats and oils C. Determination of the content of crude protein D. Determination of urea E. Determination of volatile nitrogenous bases F. Determination of amino acids (except tryptophane) G. Determination of tryptophane H. Determination of crude oils and fats I. Determination of crude fibre J. Determination of sugar K. Determination of lactose L. Determination of starch – polarimetric method M. Determination of crude ash N. Determination of ash which is insoluble in hydrochloric acid O. Determination of carbonates P. Determination of total phosphorus – photometric method Q. Determination of chlorine from chlorides Annex III – Methods of Analysis to Control the Composition of Feed Materials and Compound Feed

9. 6.12.2011ÚKZÚZ - NRL RO Praha9 Regulation 152/2009 methods of analysis Annex IV - Methods of Analysis to Control the Level of Authorised Additives in Feed A. Determination of vitamin A B. Determination of vitamin E C. Determination of the trace elements iron, copper, manganese and zinc D. Determination of halofuginone E. Determination of robenidine F. Determination of diclazuril G. Determination of lasalocid sodium Annex V - METHODS OF ANALYSIS TO CONTROL UNDESIRABLE SUBSTANCES IN FEED A. Determination of free and total gossypol B. Determination of the level of dioxins (PCDD/PCDF) and dioxin-like PCBs

10. 6.12.2011ÚKZÚZ - NRL RO Praha10 Regulation 152/2009 methods of analysis Important notes: More sensitive methods of analysis than the methods of analysis mentioned in this Annex can be used to detect the illegal presence of no longer authorised additives in feed. The methods of analysis mentioned in this Annex shall be used for confirmatory purposes. A. Determination of methyl benzoquate B. Determination of olachindox C. Determination of amprolium D. Determination of carbadox Annex VI - Methods of analysis for the determination of constituents of animal origin for the official control of feed - Conditions for the microscopic detection, identification or estimation of constituents of animal origin in feed Annex VIII - methods of analysis to control illegal presence of no longer authorised additives in feed vi - methods of analysis for the determination of constituents of animal origin for the official control of feed

11. 6.12.2011ÚKZÚZ - NRL RO Praha11 Regulation 882/2004 - Methods of sampling and analysis Sampling and analysis methods used in the context of official controls shall comply with relevant Community rules (152/2009) or, (a) if no such rules exist, with internationally recognised rules or protocols, for example those that the European Committee for Standardisation (CEN) has accepted or those agreed in national legislation; or, (b) in the absence of the above, with other methods fit for the intended purpose or developed in accordance with scientific protocols Article 11 Where paragraph 1 does not apply, validation of methods of analysis may take place within a single laboratory according to an internationally accepted protocol.

12. 6.12.2011ÚKZÚZ - NRL RO Praha12 CHARACTERISATION OF METHODS OF ANALYSIS Regulation 882/2004 – Annex III Wherever possible, methods of analysis shall be characterised by the appropriate criteria set : (a) accuracy; (b) applicability (matrix and concentration range); (c) limit of detection; (d) limit of determination; (e) precision; (f) repeatability; (g) reproducibility; (h) recovery; (i) selectivity; (j) sensitivity; (k) linearity; (l) measurement uncertainty; (m) other criteria that may be selected as required.

13. 6.12.2011ÚKZÚZ - NRL RO Praha13 Thanks for your attention www.ukzuz.cz