title: Determination of pharmaceuticals, iodinated contrast media and musk fragrances in sludge by LC/tandem MS and GC/MS.
abstract: Analytical methods have been developed that allow for the determination of antiphlogistics, lipid regulators, the antiepileptic carbamazepine, cytostatic agents, the psychiatric drug diazepam and iodinated contrast media (ICM) as well as two major polycyclic musk fragrances HHCB (galaxolide) and AHTN (tonalide) in activated and digested sludge. The procedures consist of ultrasonic solvent extraction (USE) using methanol/acetone or pressurized liquid extraction (PLE) using 100% methanol. Clean-up was performed with C18ec material and silica gel followed by LC tandem MS (electrospray or atmospheric pressure chemical ionization) detection for pharmaceuticals and iodinated contrast media as well as GC/MS in the SIM mode for musk fragrances. Absolute recoveries from spiked activated sludge in general ranged from 88+/-4 to 119+/-20% for ICM and were 78+/-15 and 87+/-10% for the AHTN and HHCB, respectively. For the pharmaceuticals, absolute recoveries in activated sludge ranged between 43 and 78%. Subsequently, compensation of losses was carried out by using surrogate standards (acidic pharmaceuticals: fenoprop, neutral pharmaceuticals: dihydro-carbamazepine, musk fragrances: AHTN-D3). With one exception the recoveries were also adequate in digested sludge ranging from 43% to 120%.
authors.affiliation: Bundesanstalt fur Gewasserkunde, Federal Institute of Hydrology (BFG), Am Mainzer Tor 1, D-56068 Kablenz, Germany. Ternes@bafg.de
authors.forename: Thomas A
authors.initials: TA
authors.lastname: Ternes
authors.forename: Matthias
authors.initials: M
authors.lastname: Bonerz
authors.forename: Nadine
authors.initials: N
authors.lastname: Herrmann
authors.forename: Dirk
authors.initials: D
authors.lastname: Löffler
authors.forename: Elvira
authors.initials: E
authors.lastname: Keller
authors.forename: Barbara Bagó
authors.initials: BB
authors.lastname: Lacida
authors.forename: Alfredo C
authors.initials: AC
authors.lastname: Alder
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D003287:Contrast Media / Q000032:analysis*; D005229:Fatty Acids, Monounsaturated / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D009812:Odorants; D004364:Pharmaceutical Preparations / Q000032:analysis*; D012722:Sewage / Q000737:chemistry*
chemical_list: D003287:Contrast Media; D005229:Fatty Acids, Monounsaturated; D004364:Pharmaceutical Preparations; D012722:Sewage; C008563:musk