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Analytical methods for substances in the Watch List under the Water Framework Directive
The JRC organised in March 2018 a technical workshop on the analysis of the existing and the three new watch list (WL) substances of the Water Framework Directive (WFD) in order to share experience and knowledge on analytical methods and to identify the obstacles to reaching the environmental quality standards (EQS) or predicted no effect concentrations (PNEC). The results from the first year of monitoring the substances of the 1st WL showed that some countries have found it very difficult to reach a satisfactory analytical limit of quantification (LOQ) for five out of the 17 substances (17-alpha-ethinylestradiol (EE2), 17-beta-estradiol (E2), azithromycin, imidacloprid, and methiocarb). The most difficult WL substance to analyse is EE2 with its very low EQS value of 0.035 ng/L. Five countries have reported for EE2 LOQs ≤ EQS, and other four countries a close LOQ (0.05 - 0.1 ng/L). However, the workshop participants (experts from Member States and Island, Switzerland and Turkey) stressed that the analysis of EE2 at ultra trace levels is complicated and work intensive because a good clean-up procedure and a very clean and sensitive LC-MS/MS instrument are necessary. The analytical methods for the three new WL substances amoxicillin, ciprofloxacin, and metaflumizone were discussed at the workshop and optimized methods for the water sample preservation and analysis for them, based on solid-phase extraction (SPE) followed by liquid chromatography triple quadrupole mass spectrometry (LC-MS/MS) analysis, are presented in this report. The workshop showed that many Member States (MS) are using today direct LC-MS/MS injection techniques. Direct LC-MS/MS injection should however only be performed for water soluble substances with low KOW and Kd(sed) values for which partitioning to suspended particulate matter (SPM) can be neglected. A literature study revealed that EE2 and E2 are strongly adsorbed to particulate matter and therefore have to be analysed in whole water samples. Moreover, around 20 % of ciprofloxacin is present in the particulate water phase. Therefore, analysis of the dissolved water phase by direct LC-MS/MS injection could deliver for this substance acceptable results similar to whole water analysis. However, an experimental analysis should be performed to confirm the comparability. Finally, some MS asked to specify in detail the different methods for the determination or calculation of the Limit of Quantification (LOQ), because the available general guidelines are not sufficient for a uniform approach. It remained unclear whether the LOQs of the presented methods are derived from appropriate real surface water samples with or without standard addition, or from calibration curves. For a better harmonisation of the methods, a consensus on the determination of the LOQ is necessary, which needs a thorough discussion on the minimum requirements for sample preparation and analysis, i.e. representative surface water matrix, standard addition, recovery, reproducibility, and multiplication factor. ; JRC.D.2-Water and Marine Resources
Analytical methods for substances in the Watch List under the Water Framework Directive
The JRC organised in March 2018 a technical workshop on the analysis of the existing and the three new watch list (WL) substances of the Water Framework Directive (WFD) in order to share experience and knowledge on analytical methods and to identify the obstacles to reaching the environmental quality standards (EQS) or predicted no effect concentrations (PNEC). The results from the first year of monitoring the substances of the 1st WL showed that some countries have found it very difficult to reach a satisfactory analytical limit of quantification (LOQ) for five out of the 17 substances (17-alpha-ethinylestradiol (EE2), 17-beta-estradiol (E2), azithromycin, imidacloprid, and methiocarb). The most difficult WL substance to analyse is EE2 with its very low EQS value of 0.035 ng/L. Five countries have reported for EE2 LOQs ≤ EQS, and other four countries a close LOQ (0.05 - 0.1 ng/L). However, the workshop participants (experts from Member States and Island, Switzerland and Turkey) stressed that the analysis of EE2 at ultra trace levels is complicated and work intensive because a good clean-up procedure and a very clean and sensitive LC-MS/MS instrument are necessary. The analytical methods for the three new WL substances amoxicillin, ciprofloxacin, and metaflumizone were discussed at the workshop and optimized methods for the water sample preservation and analysis for them, based on solid-phase extraction (SPE) followed by liquid chromatography triple quadrupole mass spectrometry (LC-MS/MS) analysis, are presented in this report. The workshop showed that many Member States (MS) are using today direct LC-MS/MS injection techniques. Direct LC-MS/MS injection should however only be performed for water soluble substances with low KOW and Kd(sed) values for which partitioning to suspended particulate matter (SPM) can be neglected. A literature study revealed that EE2 and E2 are strongly adsorbed to particulate matter and therefore have to be analysed in whole water samples. Moreover, around 20 % of ciprofloxacin is present in the particulate water phase. Therefore, analysis of the dissolved water phase by direct LC-MS/MS injection could deliver for this substance acceptable results similar to whole water analysis. However, an experimental analysis should be performed to confirm the comparability. Finally, some MS asked to specify in detail the different methods for the determination or calculation of the Limit of Quantification (LOQ), because the available general guidelines are not sufficient for a uniform approach. It remained unclear whether the LOQs of the presented methods are derived from appropriate real surface water samples with or without standard addition, or from calibration curves. For a better harmonisation of the methods, a consensus on the determination of the LOQ is necessary, which needs a thorough discussion on the minimum requirements for sample preparation and analysis, i.e. representative surface water matrix, standard addition, recovery, reproducibility, and multiplication factor. ; JRC.D.2-Water and Marine Resources
Analytical methods for substances in the Watch List under the Water Framework Directive
LOOS ROBERT (author) / MARINOV DIMITAR (author) / SANSEVERINO ISABELLA (author) / LETTIERI TERESA (author)
2018-09-14
Miscellaneous
Electronic Resource
English
DDC:
710
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