title: Combined microwave-assisted extraction and continuous solid-phase extraction prior to gas chromatography-mass spectrometry determination of pharmaceuticals, personal care products and hormones in soils, sediments and sludge.
abstract: This paper reports a sensitive analytical method based on microwave-assisted extraction and continuous solid-phase extraction (SPE), followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous determination of residues of 18 pharmaceuticals (analgesics, antibacterials, anti-epileptics, β-blockers, lipid regulators and non-steroidal anti-inflammatories), one personal care product and 3 hormones in soils, sediments and sludge. The analytes are extracted with 3:2 methanol/water under the action of microwave energy and the resulting extract is passed through a SPE column to clean up the sample matrix and preconcentrate the analytes. Then, the analytes, trapped on Oasis-HLB sorbent, are eluted with ethyl acetate, silylated and determined by GC-MS. The proposed method provides a linear response over the concentration range 2.5-20,000 ng/kg with correlation coefficients higher than 0.994 in all cases. Also, it features low limits of detection (0.8-5.1 ng/kg), good precision (within- and between-day relative standard deviation less than 7%) and recoveries ranging from 91 to 101%. The method was successfully applied to agricultural soils, river and pond sediments, and sewage sludge. All samples contained some target analyte and sludge contained most -some at considerably high concentrations.
authors.affiliation: Department of Physical and Analytical Chemistry, EPS of Linares, University of Jaén, 23700 Linares, Jaén, Spain.
authors.forename: Abdelmonaim
authors.initials: A
authors.lastname: Azzouz
authors.forename: Evaristo
authors.initials: E
authors.lastname: Ballesteros
mesh_terms: D004784:Environmental Monitoring / Q000295:instrumentation / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry; D019015:Geologic Sediments / Q000737:chemistry; D006728:Hormones / Q000032:analysis*; D008872:Microwaves; D004364:Pharmaceutical Preparations / Q000032:analysis*; D015203:Reproducibility of Results; D012722:Sewage / Q000737:chemistry; D012987:Soil / Q000737:chemistry; D012989:Soil Pollutants / Q000032:analysis*; D052616:Solid Phase Extraction; D014260:Triclosan / Q000032:analysis*
chemical_list: D006728:Hormones; D004364:Pharmaceutical Preparations; D012722:Sewage; D012987:Soil; D012989:Soil Pollutants; D014260:Triclosan