1. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Fit for Purpose - A Customers View Bernd Wenclawiak

2. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching

3. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Analytical measurements should be made to satisfy an agreed requirement

4. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Analytical measurements should be made using methods and equipment which have been tested to ensure they are fit for purpose

5. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Staff making analytical measurements should be both: qualified and competent to undertake the task and demonstrate that they can perform the analysis properly

6. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching There should be a regular independent assessment of the technical performance of a laboratory

7. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Analytical measurements made in one location should be consistent with those made elsewhere

8. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Organizations making analytical measurements should have well defined quality control and quality assurance procedures

9. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Method validation is an important requirement in the practice of chemical analysis

10. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching What is Validation?  Confirmation by examination and provision of objective evidence that the particular requirements for a specified intended use are fulfilled ISO 8402 (1994)

11. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching What is Method Validation? - 1  The process of establishing the performance characteristics and limitations of a method and the identification of the influences which may change these characteristics and to what extent.  Which analytes can it determine in which matrices in the presence of which interferences?  Within these conditions what levels of precision and accuracy can be achieved?

12. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching What is Method Validation? - 2  The process of verifying that a method is fit for purpose, i.e. for use for solving a particular analytical problem  This means the method must be suitable  Method validation is not solely the process of evaluating the performance parameters

13. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching The Method Validation Process Implies:  the use of equipment within its specifications  that the operator is fit for purpose

14. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Why is Method Validation Necessary?  Importance of analytical measurement  The professional duty of the analytical chemist

15. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching When should Methods be Validated ?  Comparing methods  Replacement of instruments  Change of operator  Other significant changes

16. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching How should Methods be Validated?  Who carries out method validation?  Deciding what degree of validation is required  The analytical requirement

17. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Choosing, Developing and Evaluating Methods Problem requiring chemical analysis: Set analytical requirement Identify existing method or develop new method Further development feasible? Evaluate method – fit for purpose as used in the laboratory Relax analytical requirement ? Develop method Analytical work proceeds Analytical requirement re-stated in terms of what has been accomplished Unable to do work – subcontract? En d Yes No Method validation consists of this evaluation stage, together with any performance parameters that may be evaluated under method development „Fit for purpose...“. Regardless of what existing performance data may be available for the method, fitness for purpose will be

18. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching How should Methods be Validated?  Who carries out method validation?  Deciding what degree of validation is required  The analytical requirement  Method Development  The different performance parameters of a method and what they show

19. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching How should Methods be Validated?  The different performance parameters of a method and what they show  Confirmation of identity and selectivity/specificity  Limit of detection  Limit of quantitation  Working and linear ranges  Accuracy  Trueness

20. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching How should Methods be Validated?  Interpreting bias measurements Measured value (laboratory mean) True value Interlaboratory mean Total bias Laboratory biasMethod bias Note: Laboratory and method biases are shown here acting in the same direction. In reality this is not always the case

21. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching How should Methods be Validated?  The different performance parameters of a method and what they show  Confirmation of identity and selectivity  Limit of detection  Limit of quantitation  Working and linear ranges  Accuracy  Trueness  Interpreting bias measurements  precision  repeatability  reproducibility  sensitivity  ruggedness or robustness  recovery

22. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching How should Methods be Validated?  The different performance parameters of a method and what they show  Confirmation of identity and selectivity  Limit of detection  Limit of quantitation  Working and linear ranges  Accuracy  Trueness  Interpreting bias measurements  precision  repeatability  reproducibility  sensitivity  ruggedness-robustness  recovery

23. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching The Tools of Validation  Blanks  reagent blanks  sample blanks  Samples/test materials  fortified materials/solutions  spiked materials  incurred materials  independently characterised materials  (Measurement) Standards  Reference Materials  Certified reference materials  Statistics  Replication

24. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Using Validated Methods  Two issues to consider:  are existing validation data adequate  is the analyst sufficiently competent can he achieve the performance level claimed in the method?

25. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Rules Recommended to Ensure Acceptable Performance  Analyst should be familiar with method before using it for the first time  Work firstly under supervision  get training  think ahead of process, solutions etc required  Make an assessment how many samples can be handled at a time  Make sure everything needed is available before work starts

26. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Using Validation Data to Design QC  Internal QC  External QC

27. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Using Validation Data to Design QC  Internal QC includes:  blanks  chemical calibrants  spiked samples  blind samples  replicate analysis  QC samples  control charts (recommended)

28. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Using Validation Data to Design QC  External QC  e.g. proficiency testing (external quality assessment)  participation in proficiency testing schemes

29. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Documentation of Validated Methods 1  When the validation process is complete document the procedures of the method (also important for auditing and evaluation purposes)  With appropriate documentation  reuse of method is more consistent  uncertainty contribution is decreased  Test quality of documentation with a competent colleague

30. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Documentation of Validated Methods 2  Standard guidance for documentation is found in ISO 78 series  “house style” is also adequate  Documented methods form an important part of a lab’s quality system  document control  is documentation complete  authorized for use  which version  which date  author  copyrights  when last updated

31. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Method Documentation Protocol

32. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Implications of Validation Data for Calculating Results and Reporting  Translate data in results to solve customers problem  Consider:  are observed differences significant? precision data for repeatability and reproducibility  Quality controls confirm method is in control based on validation data producing meaningful results  Estimation of measurement uncertainty enables expression for level of confidence

33. Wenclawiak, B.: Fit for Purpose – A Customers View© Springer-Verlag Berlin Heidelberg 2003 In: Wenclawiak, Koch, Hadjicostas (eds.) Quality Assurance in Analytical Chemistry – Training and Teaching Implications of Validation Data for Calculating Results and Reporting  The analyst needs access to validation data to support validity of results  The customer may not need or understand it  Information about uncertainties might not be understood by everybody (lawyers)  When required: uncertainty should be reported (confidence limits e.g. 95 %)