Guidance Document on Pesticide Analytical ... - ec.europa.eu

1 1 SANTE/2020/12830, 24. February 2021 Guidance Document on Pesticide Analytical Methods for Risk Assessment and Post-approval Control and Monitoring Purposes1 Supersedes Guidance Documents SANCO/3029/99 and SANCO/825/00 Version history Version Year Reasons for update SANCO/3029/99 Rev. 4 2000 Original version SANCO/825/00 Rev. 6 2000 Original version Rev. 7 2004 Minor revision Rev. 8 06/2010 Implementation of changes from Regulation (EC) No. 396/2005 and OECD (ENV/JM/ENV/JM/MONO(2007) Rev. 11/2010 Revised version SANTE/2020/12830 (combined Guidance ) 2020 Implementation of changes from Regulation (EU) No 283/2013 & 284/2013, Harmonisation of validation requirements 1 This Document has been conceived as Technical Guidelines of the Commission Services.)

2 It does not represent the official position of the Commission. It does not intend to produce legally binding effects. Only the European Court of Justice has jurisdiction to give preliminary rulings concerning the validity and interpretation of acts of the institutions of the EU pursuant to Article 267 of the Treaty. 2 1 Objective and scope .. 4 2 General items .. 6 Good Laboratory Practice .. 6 Description of an Analytical method and its validation results .. 6 Hazardous reagents .. 7 Acceptable Analytical techniques considered commonly available .. 7 Isotopically labelled internal standard (IL-IS).

3 7 Multi-residue methods .. 7 Single residue methods and common moiety methods .. 8 Derivatisation .. 9 Hydrolysis .. 9 Methods for isomeric mixtures .. 9 3 Method validation parameters ..10 Matrix effects ..10 Calibration ..10 Limit of detection ..12 Limit of quantification ..12 Recovery and repeatability ..12 Selectivity and specificity ..13 Confirmation ..14 Confirmation simultaneously to primary detection ..14 Confirmation by an independent Analytical technique ..14 Independent laboratory validation (ILV) ..15 Extract and standard stability.

4 16 Final extract stability ..16 Standard stability ..16 Extraction efficiency ..16 Availability of standards ..16 4 Validation requirements for quantitative methods for risk assessment ..17 Validation requirements for methods for risk assessment ..17 Selection of analytes ..18 Samples ..18 Validation requirements ..20 Validation requirements for Analytical methods in physical and chemical properties determination ..21 Minimum validation requirement for the assessment of existing methods for risk assessment ..22 5 Validation requirements for methods for post-approval control and monitoring purposes 23 Analytical methods for monitoring residues in food of plant Selection of analytes.

5 23 Commodities and matrix groups ..23 Limit of Independent laboratory validation (ILV) ..24 Confirmation ..24 Analytical methods for monitoring residues in food of animal origin ..25 Selection of analytes ..25 Commodities ..25 Limit of Independent laboratory validation (ILV) ..25 Confirmation ..25 3 Analytical methods for monitoring residues in soil ..26 Selection of analytes ..26 Samples ..26 Limit of Confirmation ..27 Analytical methods for monitoring residues in water ..28 Selection of analytes ..28 Samples.

6 28 Limit of Direct Independent laboratory validation (ILV) ..29 Confirmation ..29 Analytical methods for monitoring residues in air ..30 Selection of analytes ..30 Samples ..30 Limit of Sorbent characteristics ..30 Further validation data ..30 Confirmatory methods ..31 Analytical methods for monitoring residues in body fluids and tissues ..32 Selection of analytes ..32 Samples ..32 Limit of Confirmation ..32 6 Abbreviations ..33 7 References ..35 Appendix 1: List of commodities and their respective matrix groups (adopted from EFSA PROFile ).

7 37 Appendix 2: List of methods required ..50 4 1 Objective and scope This Document provides Guidance to applicants, Member States and EFSA on the validation requirements and assessment for quantitative Pesticide Analytical methods for risk assessment and post-approval control and monitoring purposes (thereafter called risk assessment methods and monitoring methods ) under section of Annex II of Regulation (EC) No 1107/2009 [1] and of the provisions laid down in sections and of Regulation (EU) No 283/2013 [2], as well as of sections and of Regulation (EU) No 284/2013 [3].

8 It also applies to applications for setting or modification of a maximum residue level (MRL) within the scope of Regulation (EC) No 396/2005 [4]. This Guidance can also be used for active substances approved under the old data requirements according to Regulation (EC) No 544/2011 [5], new MRL applications, MRL reviews, and product authorisations for these substances. Deviations shall be justified with SANTE/11509/2013 rev. [6]. It is not intended for biological agents such as bacteria, fungi or viruses. Risk assessment methods are required to support studies on environmental fate efficacy mammalian toxicology operator, worker, resident and bystander exposure residues in plants and animal commodities, processed food commodities and feed ecotoxicology physical and chemical properties Analytical methods used for determination of physical and chemical properties have been included in this Guidance Document for completeness reasons.

9 However, it has to be noted that the matrix used in these tests is considerably less complex, usually only consisting of water, buffer solution or organic solvent and the substance to be determined. Moreover, the analyte concentration used in the Analytical methods for physical and chemical properties is often considerably higher than in the other methods for risk assessment. Monitoring methods are required to enable Member States to determine compliance with established MRLs in or on food of plant and animal origin, but also for monitoring purposes in soil, water (drinking-, ground- and surface water), air and body fluids and tissues.

10 For further matrices such as animal feed and fish matrices, there is currently no requirement for monitoring methods, since MRLs have not been set in Regulation (EC) No 396/2005 yet. In this Guidance it is recognised that there will be overlap between requirements for risk assessment and monitoring methods, supporting both. Therefore, requirements have been harmonised where possible. This Guidance Document supersedes SANCO/3029/99-rev. 4. and SANCO/825/00-rev. It also has been elaborated in consideration of OECD ENV/JM/MONO(2007)17 ( Guidance 5 Document on Pesticide residue Analytical methods) [7] and SANTE/12682/2019 ( Guidance Document on Analytical quality control and method validation procedures for Pesticide residues and analysis in food and feed) [8].