Spring in the Bridger Mountains

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

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

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

Outline Method Selection Method Validation Montana Examples

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

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

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

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

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

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

Validation Support with evidence Prove validity Authenticate

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

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)

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

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

Lasalocid Confirmation Data Date Analyzed AAFCO Sample ID Sample Type AAFCO National Ranges (g/T) Montana Results (g/T) 4/21/ Cattle Grower Medicated /21/ /29/ /29/ /1/ Average RSD (%) 0.65

Monensin Confirmation Data Date Analyzed AAFCO Sample ID Sample Type AAFCO National Range (g/T) Montana Results (g/T) 1/27/ Pelleted Beef Spec /2/ /19/ /10/ /25/ /7/ /7/ /7/ Average RSD (%) 3.45

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

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

Acknowledgements Dan Singer Robin Johnson Cara Robertus Jona Verreth

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

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