Critical Literature Review of Analytical Methods Applicable To
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FINAL REPORT Reference: PFA.750.011.001 Date: February 2021 Critical literature review of analytical methods applicable to environmental fate studies Critical literature review of analytical methods applicable to environmental fate studies Report number: PFA. 750.011.001 NOTICE This report was commissioned by the European Chemicals Agency (ECHA). The author of the report, Peter Fisk Associates Limited, accepts no liability for loss or damage resulting from reliance on the contents of this report by any third party. This report does not necessarily reflect the official opinion of ECHA or the European Commission. ECHA and the European Commission do not guarantee the accuracy or correctness of the information included in this report. Neither ECHA or the European Commission, nor any person acting on their behalf, may be held responsible or liable for any reliance or use of the information contained in this report. Wood environment and infrastructure solutions UK Client limited (for ECHA under Framework ECHA/2015/50) Client’s reference ECHA/2019/236 This report is issued by Peter Fisk Associates Limited, Saxon House, John Roberts Business Park, Pean Hill, Whitstable, Kent CT5 3BJ. Company Number 05758319. Tel. +44 1227 470901, web www.pfagroup.eu AUTHORISATION RECORD Conclusions drawn and recommendations made in this report represent the unbiased view of Peter Fisk Associates Limited on the basis of the data presented and obtained. The name below confirms that this version of the report is complete and final. Name Oliver Warwick Director Position Peter Fisk Associates Limited Date 11 February 2021 Peter Fisk Associates Limited operates a business management system certified to ISO 9001, 14001 and 27001 for the provision of consultancy services to international clients on the assessment and management of the exposure, hazards and risks of industrial, professional and consumer products in the EU and UK regulatory context. Created in PFA Limited Report Template, Version 9, 13 January 2021 Page ii Report Template Version 9, 13th January 2021 Critical literature review of analytical methods applicable to environmental studies 3 Table of Contents 1. ABSTRACT..................................................................................................... 11 2. INTRODUCTION ............................................................................................ 12 3. REQUIREMENTS FOR REGULATORY COMPLIANCE AND TEST VALIDITY ........ 14 3.1 Existing regulatory guidance for the design and interpretation of bioaccumulation studies ....................................................................................................... 18 3.1.1 Acceptable test systems .......................................................................................... 18 3.1.2 Requirements for use of radiolabelled test substance ................................................... 19 3.1.3 Recommendations in relation to sampling/clean-up, extraction and analysis ................... 19 3.1.4 Requirement for the identification of metabolites ........................................................ 20 3.2 Comparison of test guidelines for bioaccumulation studies .................................. 20 3.3 Existing regulatory guidance for design and interpretation of degradation simulation studies (surface water, sediment, and soil) ..................................................... 24 3.3.1 Requirements for use of radiolabelled test substance ................................................... 25 3.3.2 Identification of transformation/degradation products .................................................. 25 3.3.3 Simulation study test temperature ............................................................................ 26 3.3.4 Requirement to conduct further studies ..................................................................... 26 3.3.5 Analytical methodology ............................................................................................ 27 3.4 Comparison of test guidelines for degradation simulation studies ......................... 27 3.5 Conclusions on the regulatory requirements for bioaccumulation and degradation simulation studies ....................................................................................... 34 4. METHODOLOGY OF THE LITERATURE SEARCH .............................................. 35 4.1 Current state of the science for environmental fate studies ................................. 35 4.1.1 Keywords and information sources ............................................................................ 35 4.1.2 Inclusion and exclusion criteria ................................................................................. 36 4.1.3 Quality criteria ........................................................................................................ 36 4.1.4 Insights from EFSA Draft Assessment Reports ............................................................ 37 4.1.4.1 Plant Protection Products (PPP, ‘Pesticides’) Literature ........................................................... 37 4.1.4.2 European Food Safety Authority (EFSA) DARs for PPPs .......................................................... 38 4.1.4.2.1 Searching DARs ..................................................................................................................... 38 4.1.4.2.2 Active substances assessed. .................................................................................................... 39 4.2 Insights from related areas: challenges and techniques ...................................... 40 4.2.1 Introduction ........................................................................................................... 40 4.2.2 Keywords for literature searching .............................................................................. 40 4.2.3 Inclusion and exclusion criteria ................................................................................. 41 4.2.4 Outcome of the literature search ............................................................................... 42 4.2.5 Additional sources ................................................................................................... 46 4.2.6 Criteria for review of literature sources ...................................................................... 47 PETER FISK ASSOCIATES LTD VERSION 2 (05/12/2016) 4.3 Guidelines for validation of analytical methods .................................................. 48 4.3.1 Keywords and information sources ............................................................................ 48 4.4 In silico tools for prediction of transformation and degradation products ............... 48 4.4.1 Keywords and information sources ............................................................................ 48 5. FINDINGS ON CURRENT PRACTICE IN GUIDELINE BIOACCUMULATION AND PERSISTENCE STUDIES ............................................................................... 49 5.1 Analytical methods used in fish bioaccumulation testing (OECD 305) ................... 49 5.2 Analytical methods used in persistence testing in soil (OECD 307) ....................... 60 5.3 Analytical methods used in persistence testing in sediment (OECD 308) ............... 65 5.4 Analytical methods used in persistence testing in water (OECD 309) .................... 71 5.5 Isotopic Labelling Methods Recommended in OECD 305, 307, 308 and 309 .......... 74 5.6 Isotopic Labelling Analysis Methods Used in European Food Safety Authority (EFSA) Draft Assessment Reports (DARs) for PPPs ..................................................... 75 6. KEY ASPECTS TO CONSIDER PRIOR TO CONDUCTING BIODEGRADATION AND BIOACCUMULATION STUDIES ..................................................................... 83 6.1 Characterisation of the substance .................................................................... 83 6.2 Key physico-chemical properties of the test substance: Water solubility ............... 83 6.3 In silico methods ........................................................................................... 85 6.4 Artefact formation ......................................................................................... 86 6.4.1 Artefacts in Mass Spectrometry ................................................................................ 86 6.4.2 Artefact formation and contamination from sampling and sample preparation ................. 86 6.4.3 Radiolysis .............................................................................................................. 87 6.4.4 Contamination of the solvent .................................................................................... 88 6.4.5 Improper storage of samples .................................................................................... 88 6.4.6 Contamination from glassware, external media or instrumentation ................................ 89 6.5 Calibration and Internal Standards ................................................................... 89 6.6 Quality criteria and method validation .............................................................. 90 6.6.1 Current guidelines on quality criteria for analytical methods in environmental fate studies 90 6.6.2 Guidelines for validation of analytical methods used in other fields ................................ 91 7. SAMPLE HANDLING AND EXTRACTION ......................................................... 99 7.1 Sampling .....................................................................................................