Analysis of musk fragrances in environmental samples

The methods for the determination of polycyclic and nitro-aromatic musk compounds in comparison to other fragrances such as OTNE ([1,2,3,4,5,6,7,8-octahydro-2,3,8,8-tetramethylnaphthalen-2yl] ethan-1-one) as well as those for the respective metabolites are described in this contribution. It covers instrumental aspects, as well as procedures for extraction and clean-up. Protocols for the determination of musks in water, sludge, biota, and air are summarised and discussed. Extractions by means of solid phase extraction (SPE) and liquid-liquid extraction (LLE) in case of water samples are evaluated for the diverse applications, i.e., wastewater, surface water and seawater. While LLE is preferred for the analysis of bulk for transport studies and for special process studies SPE might be worth the effort. Considering sludge, sediment and biota samples, drying and successive accelerated solvent extraction. Soxhlet extractions as well as cold column extractions are being compared. ASE has proven to be the most exhaustive and quickest to adopt method. Clean-up by means of size exclusion chromatography and silica sorption chromatography with their respective merits and problems are demonstrated. Suggestions for routine and research analysis are also given. The diverse approaches for enantioselective separations are discussed in respect to HHCB, AHTN and the metabolite HHCB-lactone. The power of two-dimensional (GCxGC) approaches is demonstrated considering the various production impurities (isomers) of the two polycyclic musks with the highest usage rates. The usage of tandem mass spectrometry and high resolution mass spectrometry for the same purpose is also discussed. The identification of an isomer of the HHCB-transformation product HHCB-lactone from wastewater treatment that has not been described in the literature before, is presented as well. Additionally some ideas to make the REACh process more efficient are discussed considering the special experiences from the development of the analysis of musk fragrances in the environment.