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SID 5 Research Project Final Report General enquiries on this form should be made to: Defra, Science Directorate, Management Support and Finance Team, Telephone No. 020 7238 1612 E-mail: [email protected] SID 5 Research Project Final Report Note In line with the Freedom of Information Act 2000, Defra aims to place the results Project identification of its completed research projects in the public domain wherever possible. The 1. Defra Project code PS2515 SID 5 (Research Project Final Report) is designed to capture the information on the results and outputs of Defra-funded 2. Project title research in a format that is easily PS2515 Specific additional Analytes - Development and publishable through the Defra website. A Validation of Methods for Specific Analytes Required in SID 5 must be completed for all projects. Support of the Pesticide Residues Committee (PRC) • This form is in Word format and the Annual Surveilance Programme boxes may be expanded or reduced, as appropriate. 3. Contractor Central Science Laboratory ACCESS TO INFORMATION organisation(s) Sand Hutton The information collected on this form will York be stored electronically and may be sent to any part of Defra, or to individual YO41 1LZ researchers or organisations outside Defra for the purposes of reviewing the project. Defra may also disclose the information to any outside organisation 54. Total Defra project costs £ 177,577 acting as an agent authorised by Defra to (agreed fixed price) process final research reports on its behalf. Defra intends to publish this form 5. Project: start date ................ 01 April 2004 on its website, unless there are strong reasons not to, which fully comply with exemptions under the Environmental end date ................. 31 March 2007 Information Regulations or the Freedom of Information Act 2000. Defra may be required to release information, including personal data and commercial information, on request under the Environmental Information Regulations or the Freedom of Information Act 2000. However, Defra will not permit any unwarranted breach of confidentiality or act in contravention of its obligations under the Data Protection Act 1998. Defra or its appointed agents may use the name, address or other details on your form to contact you in connection with occasional customer research aimed at improving the processes through which Defra works with its contractors. SID 5 (Rev. 3/06) Page 1 of 16 6. It is Defra’s intention to publish this form. Please confirm your agreement to do so.................................................................................... YES NO (a) When preparing SID 5s contractors should bear in mind that Defra intends that they be made public. They should be written in a clear and concise manner and represent a full account of the research project which someone not closely associated with the project can follow. Defra recognises that in a small minority of cases there may be information, such as intellectual property or commercially confidential data, used in or generated by the research project, which should not be disclosed. In these cases, such information should be detailed in a separate annex (not to be published) so that the SID 5 can be placed in the public domain. Where it is impossible to complete the Final Report without including references to any sensitive or confidential data, the information should be included and section (b) completed. NB: only in exceptional circumstances will Defra expect contractors to give a "No" answer. In all cases, reasons for withholding information must be fully in line with exemptions under the Environmental Information Regulations or the Freedom of Information Act 2000. (b) If you have answered NO, please explain why the Final report should not be released into public domain Executive Summary 7. The executive summary must not exceed 2 sides in total of A4 and should be understandable to the intelligent non-scientist. It should cover the main objectives, methods and findings of the research, together with any other significant events and options for new work. Background The Pesticide Residues Committee (PRC) coordinates an annual programme for the monitoring of pesticide residues in the UK food supply. One of the goals of the monitoring is to ensure that pesticides are being used in accordance with good agricultural practice so that consumers are not exposed to harmful levels of pesticide residues. The analytical methods that underpin the monitoring programme must provide accurate information on the concentrations of pesticide residues in a wide range of foodstuffs and must satisfy the requirements of statutory Maximum Residue Levels (MRL’s). This is a challenging task because the analytical requirements are constantly evolving due to the development and introduction of new pesticides and because of ongoing changes in the legislation. Therefore it is vital that; (i) New analytical methods are developed for new pesticides and (ii) More efficient methods are developed to reduce analytical costs and increase the scope of pesticide testing. Wherever possible an attempt is made to incorporate the analysis of new pesticides into multi- residue, rather than single residue methods. Since 2006 it has become a requirement to collaborate with the newly formed European Union Community Reference Laboratories (CRLs) to avoid unnecessary duplication of effort. Main objectives The primary purpose of this research is to support the necessary ongoing development of the UK pesticides monitoring programme by providing the Pesticide Residues Committee (PRC) with robust, rapid and lower cost methods for the analysis of pesticide residues in foods. During the period 2004 - 2007 the Pesticide Safety Directorate (PSD) identified the need to develop methods for 35 pes ticide/commodity combinations not previously included in the PRC SID 5 (Rev. 3/06) Page 2 of 16 programme. PSD also requested the development of improved methods for a number of pesticides including; amitraz, butacarboxim, cymoxanil, fluazinam, propamocarb, trinexapac ethyl and a group of ‘difficult analytes’ (captafol, captan, chlorothalonil dichlofluanid, dicofol, folpet and tolylfluanid). Summary of research findings Single Residue Analytes Five single residue methods were evaluated/developed. These included procedures for amitraz, fosetyl-aluminium, metam sodium, sulphuryl fluoride and trinexapac-ethyl. A new method for the determination of amitraz (determined as the 2,4-dimethylaniline moiety) in apples, pears and strawberries, based on hydrolysis, liquid/liquid extraction (LLE) and gas chromatography mass spectrometry (GC-MS) was successfully developed, validated and published in the peer reviewed literature [1]. Using a single LLE step, mean recoveries of 61 – 73 % [Coefficient of Variations (CVs) of 4 – 11 %] were considered acceptable for screening. With the introduction of a second LLE step, improved recoveries in the range of 71 – 96 % (CVs 3 – 9 %) were considered suitable for quantification. The method, which was successfully validated at 0.02 and 0.10 mg kg -1 in a range of commodities, is a lower cost rapid alternative to the registration method and was employed in the 2006 monitoring programme. A published liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure [2] for the determination of fosetyl-aluminium in lettuce was evaluated. The limit of quantification was relatively poor at 2.0 and 10.0 mg kg -1 for apples and lettuce respectively. Although the mean recovery during validation was 79 % (CV of 8 %) at 2.0 mg kg -1 in apples, further work is required before the method can be considered for use in the PRC programme. Fosetyl- aluminium was not compatible with the generic acetonitrile extraction procedure [3] and the Community Reference Laboratory for single methods was not able to provide an alternative method. The established GC method for the determination of dithiocarbamates (after conversion to CS 2) [4] was successfully validated for the determination of metam sodium at 0.02 – 0.05 mg kg -1 in strawberries and 0.1 – 1.0 mg kg -1 in lettuce. An evaluation of the registration method for sulphuryl fluoride concluded that the method was not suitable for routine analysis and would be expensive to implement in the PRC programme. A published LC-MS/MS procedure for the determination of trinexapac as trinexapac free acid [5] was successfully validated at 0.02 and 0.10 mg kg -1 in wheat and subsequently used for PRC monitoring in 2006. Trinexapac free acid was not compatible with the generic QuEChERS (QUick Easy Cheap Effective Rugged and Safe) acetonitrile extraction procedure [3]. ‘Difficult’ analytes A method based on generic buffered QuEChERS acetonitrile extraction [6] with dispersive solid phase cleanup in combination with a programmable thermal vaporisation injector and low pressure gas chromatography tandem quadrupole mass spectrometry (PTV-LP-GC-MS/MS) was successfully validated for captan, dichlofluanid, folpet, and tolylfluanid at 0.02 mg kg -1 in apples. These pesticides tend to degrade during conventional capillary GC analysis, and have caused analytical difficulties for laboratories contributing to PRC surveillance. The method developed was also suitable for screening captafol and chlorothalonil at 0.01 mg kg -1 . The results demonstrate that PTV-LP-GC-MS/MS is a useful technique for the “difficult” analytes that are prone to thermal degradation. However, further work is required to optimize the methods for dicofol and chlorothalonil, and to test the robustness and reliability
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