title: Determination of petroleum contamination in shellfish using solid phase micro-extraction with gas chromatography-mass spectrometry.
abstract: Headspace solid phase micro-extraction (HS-SPME) has been applied as a sampling technique for the determination of petroleum contamination in shellfish using capillary gas chromatography-mass spectrometry (GC-MS). A poly(dimethylsiloxane) fused silica fibre (100 microm thickness) was found to be satisfactory for the extraction of a range of aliphatic hydrocarbons (HCs) from homogenised shellfish tissues. The SPME conditions, including temperature, salt content, extraction time and desorption temperature, were optimised for a range of aliphatic HCs (C9-C20). A methyl silicone column GC (12 m x 0.20 mm, 0.33 microm layer thickness) was used with a temperature programme from 40 to 260 degrees C and the HCs were determined within a mass range of m/ z=50-550 in electron impact mode. Calibration range was from 10 to 5000 ng/g with linear correlation coefficients ( r(2)) of 0.982 for nonane to 0.997 for octadecane. Detection limits for aliphatic HCs, spiked into shellfish (mussel) tissues, varied from 3.6 ng/g (tetradecane) to 51 ng/g (eicosane) and relative standard deviation (% RSD) values ranged from 1.4% (hexadecane) to 24.3%(eicosane).
authors.affiliation: Ecotoxicology Research Unit, Department of Chemistry, Cork Institute of Technology, Bishopstown, Cork, Ireland. mstackenvdept@eircom.net
authors.forename: Mary A
authors.initials: MA
authors.lastname: Stack
authors.forename: Sharon
authors.initials: S
authors.lastname: O'Connell
authors.forename: Kevin J
authors.initials: KJ
authors.lastname: James
mesh_terms: D000818:Animals; D002138:Calibration; D004784:Environmental Monitoring; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010578:Petroleum / Q000032:analysis*; D012680:Sensitivity and Specificity; D012758:Shellfish / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D010578:Petroleum; D014874:Water Pollutants, Chemical