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.

作者: Abdelmonaim Azzouz , Evaristo Ballesteros

DOI: 10.1016/J.SCITOTENV.2011.12.058

关键词:

摘要: This paper reports a sensitive analytical method based on microwave-assisted extraction and continuous solid-phase (SPE), followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous determination of residues 18 pharmaceuticals (analgesics, antibacterials, anti-epileptics, β-blockers, lipid regulators non-steroidal anti-inflammatories), one personal care product 3 hormones in soils, sediments sludge. The analytes are extracted with 3:2 methanol/water under action microwave energy resulting extract is passed through SPE column to clean up sample matrix preconcentrate analytes. Then, analytes, trapped Oasis-HLB sorbent, eluted ethyl acetate, silylated determined GC-MS. proposed provides linear response over concentration range 2.5-20,000 ng/kg correlation coefficients higher than 0.994 all cases. Also, it features low limits detection (0.8-5.1 ng/kg), good precision (within- between-day relative standard deviation less 7%) recoveries ranging from 91 101%. was successfully applied agricultural river pond sediments, sewage All samples contained some target analyte sludge most -some at considerably high concentrations.

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