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