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Non-Target Screening ‒ a Powerful Tool for Selecting Environmental Pollutants

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Non-Target Screening ‒ a Powerful Tool for Selecting Environmental Pollutants RAPPORT M-27/2013 Non-target screening – A powerful tool for selecting environmental pollutants Non-target screening - A powerful tool for selecting environmental pollutants (M-27/2013) Preface NILU in collaboration with UmU was engaged by The Norwegian Climate and Pollution Agency (Klif) to perform a new type of screening project which was called “non specific” or “non target” screening. The main goal with this project was to test the potential and practicalness of the available non-target screening methods for identification of unknown or new emerging environmental pollutants. It was also desired to try to estimate the quantity of the identified compounds. Kjeller, Mars 2013 Martin Schlabach Seniorforsker, Miljøkjemi 2 Non-target screening - A powerful tool for selecting environmental pollutants (M-27/2013) 3 Non-target screening - A powerful tool for selecting environmental pollutants (M-27/2013) Contents Preface .......................................................................................................... 2 Contents ......................................................................................................... 4 1. Summary ..................................................................................................... 6 2. Sammendrag ................................................................................................. 8 3. Introduction ............................................................................................... 10 4. Theoretical background ................................................................................. 12 4.1 Principles of compound identification by mass spectrometry .............................. 12 4.2 Use of chromatographic methods for separation and structural information ........... 13 4.3 Limitations .......................................................................................... 15 5. Methods .................................................................................................... 16 5.1 Sampling ............................................................................................. 16 5.2 Sample extraction .................................................................................. 16 5.2.1 Wastewater influent/effluent and influent particle ................................. 16 5.2.2 Sediment and sludge ....................................................................... 16 5.2.3 Biota samples ............................................................................... 17 5.3 GCxGC-MS and GC-HRMS methods ............................................................... 17 5.3.1 Sample pretreatment ...................................................................... 17 5.3.2 Instrumental analysis methods ........................................................... 17 5.3.3 Data treatment ............................................................................. 17 5.4 LC-MS analyses ...................................................................................... 18 5.4.1 Sample pretreatment ...................................................................... 18 5.4.2 Instrumental analysis methods ........................................................... 18 5.4.3 Data treatment ............................................................................. 18 6. Results and Discussion ................................................................................... 19 6.1 General overview of results ...................................................................... 19 6.2 Identified compounds of special interest ...................................................... 20 6.2.1 PPCP .......................................................................................... 20 6.2.2 PACs........................................................................................... 21 6.2.3 Additives ..................................................................................... 21 6.2.4 Phthalates/adipates ....................................................................... 21 6.2.5 Pesticides .................................................................................... 21 6.2.6 Halogenated compounds .................................................................. 22 6.3 Sample characteristics ............................................................................ 23 6.3.1 Air samples .................................................................................. 23 6.3.2 Samples from sewage treatment plant ................................................. 23 6.3.3 Sediment sample ........................................................................... 23 4 Non-target screening - A powerful tool for selecting environmental pollutants (M-27/2013) 6.3.4 Biota samples ............................................................................... 24 7. Conclusions and recommendations .................................................................... 25 8. References ................................................................................................. 26 Appendix ...................................................................................................... 28 Remote air GC-MS ........................................................................................ 30 Remote air LC-MS ......................................................................................... 31 Urban air GC-MS .......................................................................................... 42 Urban air LC-MS ........................................................................................... 44 Digested sludge GC-MS .................................................................................. 53 Digested sludge LC-MS ................................................................................... 57 Raw sludge GC-MS ........................................................................................ 68 Raw sludge LC-MS......................................................................................... 75 Influent GC-MS ............................................................................................ 78 Influent LC-MS ............................................................................................. 82 Influent particles GC-MS................................................................................. 92 Influent particles LC-MS ................................................................................. 94 Effluent GC-MS ........................................................................................... 104 Effluent LC-MS ........................................................................................... 107 Contaminated fjord GC-MS ............................................................................ 122 Contaminated fjord LC-MS ............................................................................. 128 Prawns GC-MS ............................................................................................ 136 Prawns LC-MS ............................................................................................. 138 Cod liver GC-MS .......................................................................................... 150 Cod liver LC-MS .......................................................................................... 151 Common eider GC-MS ................................................................................... 156 Common eider LC-MS ................................................................................... 157 Common shag GC-MS .................................................................................... 165 Common shag LC-MS .................................................................................... 166 Herring gull GC-MS ...................................................................................... 175 Herring gull LC-MS ....................................................................................... 177 5 Non-target screening - A powerful tool for selecting environmental pollutants (M-27/2013) 1. Summary This study applies the new non-target screening technique that means the identification of environmental pollutants without a preceding selection of the compounds of interest. Analysis of complex mixtures in environmental samples is an extremely difficult task. Since sample matrices in most cases are complex, traditionally ultra trace analytical methods were specifically developed for a certain type of sample and group of substances. This traditional targeted approach gives good sensitivity and reliable identification and quantification of the target compounds, and has been used with success for several decades. However, this traditional approach has a significant drawback as it always will miss all compounds which were not selected at the start of the analyses, that means normally all unknowns or other untargeted substances even in high concentrations or with severe toxic potential. There are good reasons to believe that the concentration of the unknowns or unidentified compounds exceeds by fare the concentration of the known’s. In addition effect studies have shown in many cases that the concentrations of the known compounds are not high enough to explain some of the toxic potentials of samples. To fill this knowledge gap non-target screening methods are very important tools for environmental chemistry. During the last decade new analytical hardware and software tools have been developed which make
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