title: Enantioselective determination of the organochlorine pesticide bromocyclen in spiked fish tissue using solid-phase microextraction coupled to gas chromatography with ECD and ICP-MS detection.
abstract: A method for enantioselective determination of bromocyclen enantiomers in fish tissue has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (CP-Chirasil-Dex CB) and a temperature program from 50 degrees C (held for 1 min), raised to 140 degrees C at 40 degrees C min(-1) and then raised at 0.2 degrees C min(-1) to 155 degrees C. This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on solid-phase microextraction (SPME). Under SPME optimized conditions, precision, linearity range and detection limits of the developed SPME-enantioselective GC procedure were evaluated and compared using two different detection systems: a classical electron-capture detection (ECD) and an element specific detection using inductively coupled plasma mass spectrometry (ICP-MS). The SPME-GC-ECD method exhibited an excellent sensitivity, with detection limits of 0.2 ng L(-1) for each enantiomer of bromocyclen. Although ICP-MS offered poorer detection limits (7 ng L(-1) as Br, equivalent to 36 ng L(-1) of each enantiomer) than conventional ECD detector, it proved to be clearly superior in terms of selectivity. The relative potential and performance of the two compared methods for real-life analysis has been illustrated by the determination of enantiomers of bromocyclen in spiked tissue extracts of trout.
authors.affiliation: Department of Physical and Analytical Chemistry, University of Oviedo, C/Julian Clavería 8, 33006 Oviedo, Spain.
authors.forename: Natalia
authors.initials: N
authors.lastname: Fidalgo-Used
authors.forename: Maria
authors.initials: M
authors.lastname: Montes-Bayón
authors.forename: Elisa
authors.initials: E
authors.lastname: Blanco-González
authors.forename: Alfredo
authors.initials: A
authors.lastname: Sanz-Medel
mesh_terms: D000818:Animals; D001643:Bridged Bicyclo Compounds / Q000032:analysis / Q000737:chemistry*; D002849:Chromatography, Gas / Q000379:methods; D005399:Fishes; D006843:Hydrocarbons, Chlorinated / Q000032:analysis / Q000737:chemistry*; D013058:Mass Spectrometry / Q000379:methods; D009132:Muscles / Q000737:chemistry; D010575:Pesticides / Q000737:chemistry*; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction; D013237:Stereoisomerism
chemical_list: D001643:Bridged Bicyclo Compounds; D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; C066635:bromocyclen