daniele sohier aoac and iso 16140 validation studies current harmonization schemes to comply with th
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AOAC ValidationTRANSCRIPT
2012
AOAC and ISO 16140 validation studies
Current harmonization schemes to comply with the stakeholders’ needs
2012
How to select a method ?
1. Validation studies: current harmonization scheme 2. Method validation and regulation requirements 3. Why do we move for method verification guidelines ?
Practicability
ISO 16140 validation AOAC validation
Training
Practicability ISO 16140 validation AOAC validation Training
2012
How to select a method ?
1. Validation studies: current harmonization scheme 2. Method validation and regulation requirements 3. Why do we move for method verification guidelines ?
Practicability
ISO 16140 validation AOAC validation
Training
Practicability ISO 16140 validation AOAC validation Training
2012
Current Guidelines & Standards
AOAC INTERNATIONAL Methods Committee Guidelines for Validation of Microbiological Methods for Food and Environmental Surfaces (2012)
ISO 16140 Standard (2002): Microbiology of food and animal feeding stuffs — Protocol for the validation of alternative method
Technical protocols for the performances assessment ► Qualitative methods ► Quantitative methods
The performances of the alternative method demonstrates or estimates the same analyte as it is measured by the corresponding reference method
2012
Current Guidelines & Standards
Categories Types Matrices (samples)
Meat products
Raw Meat cuts, carpaccio’s, minced meat…
Heat processed
Cooked ham, cooked meat preparations…
Cured Cured ham, bacon, etc…
► Categories, types, matrices… « A brain teaser! »
AOAC-RI Guidelines – PTM (2012)
▲ ▲
2012
Current Guidelines & Standards
Categories Types Matrices (samples)
Meat products
Raw Meat cuts, carpaccio’s, minced meat…
Heat processed
Cooked ham, cooked meat preparations…
Cured Cured ham, bacon, etc…
► Categories, types, matrices… « A brain teaser! »
ISO 16140 Standard (2002)
▲ ▲
▲
2012
Current Guidelines & Standards
AOAC-RI Guidelines – PTM (2012)
ISO 16140 Standard (2002)
Variety (10 matrices & 5 categories at least)
To claim a « full » validation: 5 categories, three food types per tested category - 4 food categories + Additional category - 5 food categories
Selected (5 matrices & 2 categories at least)
Selected categories
Food category (5 matrices at least, 1 category)
Selected matrices or types (ground beef / raw beef meat)
Categories Types Matrices (samples)
Meat products Raw Meat cuts, carpaccio’s, minced meat…
Heat processed Cooked ham, cooked meat preparations…
Cured Cured ham, bacon, etc…
► Claim
2012
Current Guidelines & Standards
Inter-laboratory study Required (results of 10 labs at least)
ISO 16140
Pure cultures
Detection limits 1 matrix/strain pair per tested category Minimum of 6 replicates providing fractional recovery, 6 negative & 6 positive controls, 1 lot Relative accuracy, specificity and sensitivity 60 individual samples per tested category
Audit & certification of the production plan(s)
To-do-list AOAC-RI (PTM) Method developer & independent lab
Inclusivity & exclusivity testing
Pure cultures
Matrix study Per tested matrix: 20 replicates providing fractional recovery, 5 negative and positive controls, 1-2 lots
Robustness, stability & lot-to-lot studies
Required
Independent lab
► Qualitative methods Combined validation studies
AOAC-OMA Validation study
2012
Current Guidelines & Standards
Inter-laboratory study Required (results of 10 labs at least)
ISO 16140
Pure cultures
Detection limits 1 matrix/strain pair per tested category Minimum of 6 replicates providing fractional recovery, 6 negative & 6 positive controls, 1 lot Relative accuracy, specificity and sensitivity 60 individual samples per tested category
Audit & certification of the production plan(s)
To-do-list AOAC-RI (PTM) Method developer & independent lab
Inclusivity & exclusivity testing
Pure cultures
Matrix study Per tested matrix: 20 replicates providing fractional recovery, 5 negative and positive controls, 1-2 lots
Robustness, stability & lot-to-lot studies
Required
To fit with the requirements of both technical protocols
Independent lab
► Qualitative methods
To fit with the upper requirements per tested matrix: 20 replicates providing fractional recovery, 6 negative & 6 positive controls.
This experimental design fits with the AOAC-RI and ISO 16140 calculation requirements
Combined validation studies
AOAC-OMA Validation study
2012
Current Guidelines & Standards
Inter-laboratory study Required (results of 10 labs at least)
ISO 16140
Pure cultures
Detection limits 1 matrix/strain pair per tested category Minimum of 6 replicates providing fractional recovery, 6 negative & 6 positive controls, 1 lot Relative accuracy, specificity and sensitivity 60 individual samples per tested category
Audit & certification of the production plan(s)
To-do-list AOAC-RI (PTM) Method developer & independent lab
Inclusivity & exclusivity testing
Pure cultures
Matrix study Per tested matrix: 20 replicates providing fractional recovery, 5 negative and positive controls, 1-2 lots
Robustness, stability & lot-to-lot studies
Required
To fit with the requirements of both technical protocols
Independent lab
► Qualitative methods
The same requirements
Up coming revised ISO 16140 standard
To fit with the upper requirements per tested matrix: 20 replicates providing fractional recovery, 6 negative & 6 positive controls.
This experimental design fits with the AOAC-RI and ISO 16140 calculation requirements
20 replicates providing fractional recovery, 5 negative & 5 positive controls.
This experimental design fits with the AOAC-RI (POD) and ISO 16140 calculation (RLOD) requirements
2012
Current Guidelines & Standards
► Quantitative methods
LOD & LOQ One pure culture (replicates)
Inter-laboratory study Required (results of 8 labs at least)
ISO 16140
Pure cultures
Linearity and sensivity study 1 matrix/strain pair per tested category, 5 contamination levels, 2-10 replicates, 1 lot Relative accuracy study 10 individual samples per tested category, 2-10 replicates
Audit & certification of the production plan(s)
To-do-list AOAC-RI (PTM) Method developer & independent lab
Inclusivity & exclusivity testing
Pure cultures
Matrix study Per tested matrix: 4 contamination levels, 5 replicates, 1-3 lots
Robustness, stability & lot-to-lot studies
Required
Independent lab
Combined validation studies
AOAC-OMA Validation study
2012
Current Guidelines & Standards
► Quantitative methods
LOD & LOQ One pure culture (replicates)
Inter-laboratory study Required (results of 8 labs at least)
ISO 16140
Pure cultures
Linearity and sensivity study 1 matrix/strain pair per tested category, 5 contamination levels, 2-10 replicates, 1 lot Relative accuracy study 10 individual samples per tested category, 2-10 replicates
Audit & certification of the production plan(s)
To-do-list AOAC-RI (PTM) Method developer & independent lab
Inclusivity & exclusivity testing
Pure cultures
Matrix study Per tested matrix: 4 contamination levels, 5 replicates, 1-3 lots
Robustness, stability & lot-to-lot studies
Required
To fit with the requirements of both technical protocols
Independent lab
To fit with the upper requirements per tested matrix:
5 contamination levels, 5-10 replicates. This experimental design fits with the AOAC-RI and ISO 16140 calculation requirements
Combined validation studies
AOAC-OMA Validation study
2012
► Quantitative methods
LOD & LOQ One pure culture (replicates)
Inter-laboratory study Required (results of 8 labs at least)
ISO 16140
Pure cultures
Linearity and sensivity study 1 matrix/strain pair per tested category, 5 contamination levels, 2-10 replicates, 1 lot Relative accuracy study 10 individual samples per tested category, 2-10 replicates
Audit & certification of the production plan(s)
To-do-list AOAC-RI (PTM) Method developer & independent lab
Inclusivity & exclusivity testing
Pure cultures
Matrix study Per tested matrix: 4 contamination levels, 5 replicates, 1-3 lots
Robustness, stability & lot-to-lot studies
Required
To fit with the requirements of both technical protocols
Independent lab
Current Guidelines & Standards
The same requirements
To fit with the upper requirements per tested matrix:
5 contamination levels, 5-10 replicates. This experimental design fits with the AOAC-RI and ISO 16140 calculation requirements
4 contamination levels, 5 replicates.
This experimental design fits with the AOAC-RI (Mean differences) and ISO 16140 (Accuracy profile) calculations
Up coming revised ISO 16140 standard
Revision of the protocol
Revision of the protocol
2012
Current & revised Guidelines & Standards
Some parts of the AOAC-RI and ISO 16140 technical protocols can be easily adapted to suit all the concerned requirements, the other parts should be considered as separated testing, providing additional information
This helps in saving materials and human resources during validation studies
Method developers Summary reports from combined validation studies may facilitate the selection of an alternative method for running routine analyses
International FBO
But But what about - the reference methods harmonization for a worldwide recognition…?! - the regulation requirements ?
2012
How to select a method ?
1. Validation studies: current harmonization scheme 2. Method validation and regulation requirements 3. Why do we move for method verification guidelines ?
Practicability
ISO 16140 validation AOAC validation
Training
Practicability ISO 16140 validation AOAC validation Training
2012
North America regulation
AOAC – Reference methods: FDA/BAM, USDA/FSIS…and ISO
Regulatory authorities in different jurisdictions often have specific requirements
– Follow the regulation bodies’ specific requirements to get a regulatory approval on the validation study claim Reference methods to be used, as well as
the matrices to be tested in the validation study FDA, Health Canada, USDA
2012
European regulation
ISO/CEN reference methods Alternative (proprietary) methods
– Validated against the related ISO/CEN reference method according to the ISO 16140 standard, or other international similar protocol
– Certified by a third party AFNOR Certification, MicroVal, NordVal
Legislation frame: conditions in the EC 2073 (2005)
2012
ISO 16140 validation
Categories: full claim, but… – Environmental, feeding and primary
production samples Sample size: usually 25 g sample
– Upper sample size Specific foods and food specialities
– Probiotic foods for instance – Raw milk cheeses for instance…!
Users Final check list in method selection
2012
How to select a method ?
1. Validation studies: current harmonization scheme 2. Method validation and regulation requirements 3. Why do we move for method verification guidelines ?
Practicability
ISO 16140 validation AOAC validation
Training
Practicability ISO 16140 validation AOAC validation Training
2012
Method verification
Important issue in methods harmonization deals with the food products themselves
– AOAC-RI ISPAM working group: harmonization in the classification of categories and types Food, feed, environmental and primary production samples AOAC, FDA, FSIS, Health Canada, ISO, Food Industries, Method Developers
ANNEX B in the revised ISO 16140 standard
2012
Method verification
Important issue in methods harmonization deals with the food products themselves
– AOAC-RI ISPAM working group: harmonization in the classification of categories and types Food, feed, environmental and primary production samples AOAC, FDA, FSIS, Health Canada, ISO, Food Industries, Method Developers
≠ challenges
Method verification Specific part in the
revised ISO 16140 standard
Chocolate Spices
Coffee Raw milk cheeses
Yellow egg
Probiotic food
Fruit concentrates Pet food
White egg
Blue cheese
2012
Method verification
To Stefano convenor of the ISO working group on
method verification – Quantitative methods ONE experimental design for the method
verification, but as well for the measurment uncertainties calculations
