1. Spring in the Bridger Mountains

2. MONTANA: METHOD SELECTION AND VALIDATION Lab Accreditation Meeting San Diego, March 10 th

3. MT Department of Agriculture Lab Analytical Chemistry Lab 8.625 FTE Montana State University Bozeman, MT ~2,500 samples per year

4. MT Department of Agriculture Lab ~1/2 Feed /Fertilizer samples ~1/2 Pesticide samples ISO 17025 Accreditation November 2014 2 Feed, 1 Fertilizer Method 0.5 FTE QAO position

6. Outline Method Selection Method Validation Montana Examples

7. Method Selection ISO General Requirements Appropriate Include instructions Up to date Deviations documented/accepted by customer

8. Method Selection Standard methods: preferred Based on published regulatory or consensus methods (examples: FDA, EPA, AOAC, ASTM) Non-Standard Methods: appropriate/validated Customer informed of method chosen

10. Standard Methods Validation provided by published standard. Confirm ability to operate standard methods May supplement with additional details

13. Lab Developed Methods Is a planned activity Assigned to qualified staff Need written procedure Validated before sample testing

14. Non-Standard Methods Customer must agree Customer requirements must be clear Purpose of testing defined Method validated before use

15. Validation Non standard methods Lab developed methods Std methods used outside their scope Modifications of std methods

16. Validation Support with evidence Prove validity Authenticate

17. Validation Extensive as necessary Record procedure used Statement: is method fit for intended use Range and accuracy meet customer’s needs

18. Data Studies Repeatability study Reproducibility study Matrix effect study Linearity study Establishment of LOD’s and LOQ’s Determination of method range Bias study (trueness)

19. Method Validation Report Summary of results Evaluation of results Acceptability criteria Conclusions

20. Montana Examples Monensin: AOAC method Lasalocid: AOAC method Confirmation study AAFCO check Samples

22. Lasalocid Confirmation Data Date Analyzed AAFCO Sample ID Sample Type AAFCO National Ranges (g/T) Montana Results (g/T) 4/21/20142013 - 31 Cattle Grower Medicated 56.68-59.2759.05 4/21/2014 58.91 4/29/2014 58.40 4/29/2014 59.14 5/1/2014 58.30 Average 58.76 RSD (%) 0.65

23. Monensin Confirmation Data Date Analyzed AAFCO Sample ID Sample Type AAFCO National Range (g/T) Montana Results (g/T) 1/27/20141325 Pelleted Beef Spec 19.125-21.67920.34 2/2/2014 20.29 2/19/2014 19.71 3/10/2014 19.96 3/25/2014 20.25 5/7/2014 21.28 5/7/2014 21.60 5/7/2014 21.37 Average 20.60 RSD (%) 3.45

24. Conclusions Method Selection/Validation so doable Most Feed testing methods: standard methods Confirmation of standard methods: easy This is NOT a stumbling block for accreditation

25. References International Standard, ISO/IEC 17025, Section 5.4 Test and calibration methods and method validation. Second edition 2005-05-15, Reference number ISO/IEC 17025:2005(E). Montana Department of Agriculture Quality Management System for ISO accredited methods

26. Acknowledgements Dan Singer Robin Johnson Cara Robertus Jona Verreth

27. “ Science does not know its debt to imagination. ” Ralph Waldo Emerson

28. MIDWEST AOAC meeting June 8-10 th 2015 Bozeman, MT SYMPOSIA: Pesticides at work in the Agriculture LAB State AG FEED LABS going ISO-Say what? Veterinary Toxicology and Mycotoxins NFTA technical presentations Food Safety: Chemistry and Microbiology Applications ICP workshop LIMS issues SPECIAL EVENTS: Vendor expo and presentations Tuesday evening social: Mountain Chalet surrounded by snowcapped mountains Casper-Helfe Memorial Golf Outing