Analytical Method Validation/ILV for determination of residues
Validation of the analytical method, or ILV of a primary method supplied by another Facility and already validated, to determine residues in plants, plant products, foodstuffs (of plant and animal origin), feedingstuffs and environmental samples.
Preliminary custom set-up
Just for the Analytical method validation, test design may includes an entirely new method set-up and optimisation or a checking/confirm of the analytical method supplied by the Sponsor or even a checking of the analytical method from reference literature.
Analytical method validation or ILV consist of:
Linearity (checked at each analytical sequence) with at least 5 concentrations of analytical standard in the appropriate range of concentrations diluted with untreated matrix extract.
Recovery and Precision with 2 Fortification levels on the untreated matrix: LOQ and 10xLOQ (or other suitable level) with 5 samples for each level
Acceptable ranges for the recovery and the precision depend on the matrix and the fortification level.
Interferences check 2 samples of untreated blank to check interferences, analytical artifacts and matrix effects: the analyte signal must be < 30% of LOQ.
where LOQ is defined as the low fortification level at which mean recovery and precision are acceptable.
LOD defined by Signal to Noise Ratio < 3.
Confirmatory analysis consists of additional MS/MS transition on:
– Linearity data (5 concentrations)
– Recovery and precision data at LOQ level (5 samples)
– Untreated blank data (1 sample)
If no additional transition is identified a confirmatory method is performed.
Additonally, the stability check of stock/working solutions and the stability check of the final extracts per matrix type can be carried out.
Study includes GLP managment and reporting.
REFERENCES AND GUIDELINES
SANCO/3029/99 rev. 4 (11/07/2000) – Residues: guidance for generating and reporting methods of analysis in support of pre-registration data requirements for Annex II (Part A, section 4) and Annex III (Part A, section 5) of Directive 91/414.
SANCO/825/00 rev. 8.1 (16/11/2010) – Guidance document on pesticide residue analytical methods.
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