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The application of Plant Protection Product (PPP) according to the GAP, follows residues determination in different matrices also for PPPs based on microorganisms, visit our Microbiology Area for more information.
Analytical method validation includes:
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.
Procedural Recovery and Precision with 2 Fortification levels on the untreated matrix: LOQ and 10xLOQ with 2 samples for each level.
Acceptable ranges for the recovery and the precision depend on the matrix.
Untreated blanks are carried out 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.
For samples analyses, each sample (treated and untreated blank) from field trials are extracted and purified once.
The analytical method used can be validated separately in another study or whithin the this study.
Additonally, the stability check of stock/working solutions and the stability check of the final extracts per matrix type can be carried out.
If necessary, it can be carried out a storage stability check according to OECD TG 506 which includes:
Recovery in the stored samples with a fortification at 10xLOQ (2 samples) and 1 untreated blank (1 sample) with samples stored at ≤ -18°C until analysis.
Procedural recoveries with a fortification of the samples at 10xLOQ (2 samples) freshly prepared on analysis.
Time points of analysis include time zero (T0) and all other time points relevant to storage period.
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.
OECD Guideline for Testing of Chemicals, No. 506 (16th October 2007) - Stability of Pesticide Residues in Stored Commodities.