Evaluation of Analytical Chemical Methods for Detection of Estrogens in the Environment

Compounds Matrix Extraction Clean-up Derivatization Separation and detection method MS system LOD (ng/l) Reference E2, E1, EE STP effluent SPE (C18 col)    -SPE (C18 col) -HPLC fraction. -LLE - GC-(EI)-MS Finnigan MAT Magnum ion trap 0.2 (17) E2, E1, EE STP effluents SPE (C18 col)    -HPLC fraction. - GC-MS Not reported 0.5-1 (111) E2, 17α-E2, E1, EE Surface and drinking water SPE (LiChrolut EN) PFBCI GC-(NCI)-MS HP 5973 MSD (Hewlett- Packard) 0.05-0.15 (112) E2, E1, EE STP effluent SPE (ENV+ col) -LLE, GCP (Biobeds SX- 3) -hydrolysis Acetic anhydride GC-(EI)-MS Not reported Not reported (59) E2, E1, EE, 17α-E2 (SS) River water and STP effluent Contineous LLE - Bis- (trimethylsilyl)triflouro- acetamide with 10% trimethylchlorosilane   GC-(EI)MS HP 5970 MSD (Hewlett- Packard) 58 (only E2) (53) E2, E3, E1, EE STP effluent SPE (LiChrolut EN/Bondesil C18 col.) Silicagel 60 MSTFA/TMSI/DTE (1000:4:2) GC-(EI)MS HP 5970B MSD (Hewlett- Packard) 1 (58) EE STP effluent SPE (Empore C18 disk) - - GC-(EI)MS Finigan Voyager 74 (113) E2, EE Surface water     SPE (C18 col. Or disk or PS- DVB col.) or - MTBSTFA GC-(EI)MS Voyager (Interscience) 50-300 (55)
LLE E2, E3, E1 STP effluent SPE (C18 col.) - Pentafluoropropionic acid anhydride GC-(EI)MS HP 5890 MSD (Hewlett- Packard) 5-10 (114) EE Tap and river water In sample acetylation on line SPE (PLRP) - Acetic anhydride GC-(EI)MS Finnigan MAT 44S 15 (115) E2, E1, EE STP influent and effluent SPE (SBD-XC disk) -SPE (C18/NH2 col.) -HPLC fraction. - GC-(EI)MS- MS Not reported 0.1-1.8 (14) E2, 17α-E2, E1, E2-17- acet, E2-17- valer. Influent and effluent SPE (C18/EN col.) Silicagel MSTFA/TMSI/DTE (1000:2:2) GC-(EI)MS- MS Varian Saturn 4 0.5-1 (18) E2, EE, E2gluc, E2sulf Surface water, STP effluent SPE (C18 disk) -Hydrolys. -HPLC fration. Heptafluorobutyric anhydride GC-(EI)MS- MS (only E2) Finnigan GCQ ion trap (ThermoQuest) 0.2-0.4 (48) E2, 17α-E2, E1, EE, glucuronides Surface and waste water SPE (SDB-XC disk) - hydrol. -SPE (C18/NH2) -HPLC -fraction. SIL A reagent GC-(EI)MS- MS Saturn IV ion trap (Varian) 0.1-2.4 (8) E2, E1, EE Reservoir and river water, SPE effluent SPE (C18 disk) - MTBSTFA with 1% TBDMCS GC-(EI)MS- MS ThermoQuest GCQ ion trap   1 (54)