Pesticide analysis - Staying vigilant as to the analysis and interpretation parameters
Monitoring of changes in contaminants and the correct exploitation of the pesticide analysis results require compliance with a standard framework at different levels.
From the sampling stage, companies follow a protocol established for all plan participants, in terms of standards to be met and sampling methods specific to the analysed matrices.
The laboratories solicited by the companies must be referenced by OQUALIM and capable of analysing a compulsory single list of 99 molecules (positive list), integrated within larger packs (200 or 500 molecules), that are specific to each laboratory according to the framework set by the conventional or organic plans. For organochlorine pesticides (Directive 2002/32/EC), despite the maximum levels expressed in mg/kg of animal feed with a humidity level of 12%, the results are entered on raw feed, in the same way as for all other pesticides that come under Regulation (EC) no. 396/2005.
The laboratories enter the results directly onto the Quality Portal, designed for standardised, effective data processing. The recent change in the portal aims to avoid data entry errors and better ensure data traceability as far as possible. This consists notably of pre-formatting that directs the choice of matrix/pesticide couple, among the couples defined in the plan and consistency controls are carried out: verification of the traceability of the data entered, consistency between the laboratory analysis report and the OQUALIM database, the laboratory profile within the Quality Portal. If the threshold is exceeded, an alert system enables OQUALIM to immediately and systematically launch an investigation into the causes and to interpret the result in view of the regulations and following criteria.
For transformed and/or composite products, for which no maximum residue limit has been defined, OQUALIM has defined specific transformation factors for certain matrices, that are considered coherent by the administration and provide an objective basis for the maximum residue limits for these products (allowed by Regulation (EC) no. 396/2005).
The “ethylene oxide” crisis recalls the importance of having standardised measures and confirms the role of the feed plan in refining the search for emerging contaminants.
Newsletter on monitoring plans_ April 2022 edition
Focus on the results of pesticide residues
Definition of the professional thresholds for the qualification of results
In addition to monitoring regulated pesticides and identifying emerging risks, OQUALIM also makes proposals on the interpretation of the results obtained.
Whilst the maximum residue limits (MRLs) are defined by regulations on conventional harvested products, there are no regulatory MRLs for products that can only be used as ingredients for feed. Regulation (EC) No 396/2005 stipulates that when MRLs for transformed and/or compound products have not been set, the applicable MRLs are those provided for the product(s) from which they are produced and indicated in appendix 1 taking into account the changes in pesticide residues due to the transformation and/or mixing process. However, whilst the regulation stipulates that specific concentration or dilution factors may be added to the list in appendix VI, nothing has been published to date.
In the absence of positioning by the Authorities on the issue, OQUALIM has proposed transfer coefficients to assess the health quality of these products within a sector approach. These coefficients were defined using the database of the German Federal Risk Analysis Institute (BfR) which compiles transformation factors. These professional qualification thresholds are publicly presented by the association each year as feedback from monitoring results, in the presence of the French Authorities. Similarly, in the absence of the publication of thresholds applicable to the organic sector, the Profession was required to establish its own result qualification rules, based on the values recommended in 2001 by the Bundesverband Naturkost Naturwaren (BNN).
Monitoring and identification of emerging risks
Pesticide residues are subject to monitoring under OQUALIM's "Conventional Feed", "Milk Replacer" and "Organic" plans. Screening of 200 or 500 molecules, including some that are specific to some feed materials, is carried out. In order to guarantee the necessary homogeneity of the research carried out, OQUALIM has defined a minimum shared list of 99 pesticides that all referenced laboratories must analyse. The laboratories supplement this list with molecules of their choice, notably allowing the identification of emerging risks.
OQUALIM's plans are reviewed each year by a group of experts that conduct a risk analysis including the latest news: regulatory monitoring, alerts, history, etc.
For example, following the upcoming ban of chlorpyrifos and chlorpyrifos methyl, monitoring for these pesticides will be reinforced, in order to obtain data on the contamination and persistence of these molecules.
In 2019, 377 analyses were carried out on conventional feed materials, representing 148,733 results, with: 99% of samples "compliant" or "to be monitored", with an increase in "to be monitored" results compared to previous years. This matter will be monitored by the expert groups responsible for managing these plans.
To date, we can conclude that feed materials generally comply with the regulations with only 1% of non-compliant samples.
Journal on monitoring plans_May 2020
Change in the analysis of pesticide residues in feed self-monitoring plans
Pesticides comprise one or several active substances designed to manage or destroy harmful and undesirable elements on animals and plants. They mainly represent insecticides, fungicides, herbicides, acaricides, growth regulators and repellents.
OQUALIM's "Feed" plan steering committee and the related working groups initiated a work in 2016 on the analysis of pesticide residues as part of pooled self-monitoring plans. This study showed the heterogeneity of the lists of molecules proposed by the referenced laboratories and the absence of certain historically detected compounds.
Wishing to retain an inter-laboratory diversity to promote the identification of emerging risks, the Feed plan steering committee decided to define a minimum common list or positive list that the laboratories will add to with their specific lists.
This positive list of 99 validated, mandatory molecules as part of the pooled self-monitoring plans was established on the basis of current regulations, the plan history, OQUALIM monitoring and laboratory feedback. In 2018, laboratory referencing was updated. The minimum list is included in an overall analytical research strategy of 200 or 500 molecules depending on the related monitoring plan.
Since the start of 2019, the new portal for the pooled self-monitoring plans includes the specificities of each referenced laboratory (molecules, quantification limits, MRL).
Journal on monitoring plans_May 2019
Oqualim laboratory referencing
45 referenced laboratories for 41 research types
Reliability and homogeneity of pooled analysis results are essential for robust plans. To achieve this, 3 key factors:
1/Referencing of Laboratories
Laboratory referencing is studied for a matrix/contaminant pair according to defined methods. The OQUALIM Laboratory Working Group validates referencing according to several criteria: Cofrac accreditations or equivalent, participation in Interlaboratory Comparison Tests (ILC), use of validated and/or standardised methods.
For certain contaminants, the Laboratory Working Group studies additional elements required for referencing in animal feed (specific method defined by animal feed regulations - Directive 2002/35/EC updated, standardised method or AFNOR validated alternative, etc).
2/ Laboratory Service Agreement
A Laboratory Service Agreement is signed between OQUALIM and the laboratory. The agreement includes specifications on requirements such as:
- Sample Management (identification and recording, conservation and analysis report)
- Analysis conditions (methods defined with LOQ, application of analysis methods defined by Directive 2002/32/CE updated for heavy metals and by EURL recommendations for dioxins and PCBDL). Integration of regulatory changes within 6 months after their publication in the European Union Official Journal.
- Delivery of results (expression, analytical time period and entering of results into the OQUALIM database).
3/ Research accuracy
Example of pesticide analysis - change in referencing to a positive list. In order to homogenise the list of pesticides detected within OQUALIM plans, a positive list was prepared based on current regulations, plan history, our monitoring and laboratory feedback. This minimum shared detection base includes around one hundred molecules for systematic research. This minimum list is then completed by the laboratories according to their COFRAC validated and accredited methods.
Monitoring report_Special 10 years edition_April 2018