title: Combined isolation and purification procedures prior to the high-performance liquid chromatographic-ion-trap tandem mass spectrometric determination of estrogens and their conjugates in river sediments.
abstract: A fast and sensitive analytical procedure has been developed for the simultaneous separation and determination of alpha-estradiol, beta-estradiol, estriol, estrone and ethynylestradiol and their sulfate, glucuronide and acetate conjugates in river sediments. The procedure includes a microwave-assisted extraction (MAE) with aqueous methanol (25:75, v/v) at 100 degrees C in 10 min, a clean-up on Oasis WAX cartridge and a high-performance liquid chromatography-ion-trap tandem mass spectrometry (HPLC-IT-MS/MS) with electrospray ionization. The recovery for each compounds ranged from 83 to 107% and the repeatability represented as RSDs ranged from 4.9 to 9.6%. The limits of detection (LODs) were down to 1 ng g(-1). The analytical performance of the method was evaluated using determination of free and conjugated estrogens in river sediments.
authors.affiliation: Department of Chemistry and Biochemistry, Mendel University of Agriculture and Forestry, Zemedelská 1, Brno CZ 61300, Czech Republic.
authors.forename: David
authors.initials: D
authors.lastname: Matejícek
authors.forename: Pavlína
authors.initials: P
authors.lastname: Houserová
authors.forename: Vlastimil
authors.initials: V
authors.lastname: Kubán
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002852:Chromatography, Ion Exchange / Q000379:methods*; D004784:Environmental Monitoring / Q000379:methods; D045166:Estradiol Congeners / Q000032:analysis / Q000737:chemistry; D004967:Estrogens / Q000032:analysis* / Q000737:chemistry; D019015:Geologic Sediments / Q000737:chemistry; D008872:Microwaves; D045483:Rivers / Q000737:chemistry*; D012989:Soil Pollutants / Q000032:analysis / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000302:isolation & purification*
chemical_list: D045166:Estradiol Congeners; D004967:Estrogens; D012989:Soil Pollutants; D014874:Water Pollutants, Chemical