spring in the bridger mountains. montana: method selection and validation lab accreditation meeting...
TRANSCRIPT
Spring in the Bridger Mountains
MONTANA: METHOD SELECTION AND VALIDATION
Lab Accreditation Meeting San Diego, March 10th
MT Department of Agriculture Lab
• Analytical Chemistry Lab
• 8.625 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 17025 Accreditation November 2014
• 2 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 AnalyzedAAFCO Sample
IDSample Type
AAFCO National
Ranges (g/T)
Montana Results (g/T)
4/21/2014 2013 - 31Cattle Grower
Medicated56.68-59.27 59.05
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
Monensin Confirmation Data
Date Analyzed AAFCO Sample ID Sample Type AAFCO National
Range (g/T)Montana Results
(g/T)
1/27/2014 1325 Pelleted Beef Spec 19.125-21.679 20.34
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
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 2005-05-15, 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 8-10th 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