title: Optimization and validation of organochlorine compounds in adipose tissue by SPE-gas chromatography.
abstract: Scientific evidence has shown an association between organochlorine compounds (OCC) exposure and human health hazards. Concerning this, OCC detection in human adipose samples has to be considered a public health priority. This study evaluated the efficacy of various solid-phase extraction (SPE) and cleanup methods for OCC determination in human adipose tissue. Octadecylsilyl endcapped (C₁₈-E), benzenesulfonic acid modified silica cation exchanger (SA), poly(styrene-divinylbenzene (EN) and EN/RP₁₈ SPE sorbents were evaluated. The relative sample cleanup provided by these SPE columns was evaluated using gas chromatography with electron capture detection (GC-ECD). The C₁₈-E columns with strong homogenization were found to provide the most effective cleanup, removing the greatest amount of interfering substance, and simultaneously ensuring good analyte recoveries higher than 70%. Recoveries > 70% with standard deviations (SD) < 15% were obtained for all compounds under the selected conditions. Method detection limits were in the 0.003-0.009 mg/kg range. The positive samples were confirmed by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). The highest percentage found of the OCC in real samples corresponded to HCB, o,p'-DDT and methoxychlor, which were detected in 80 and 95% of samples analyzed respectively.
authors.affiliation: Requimte, Instituto Superior de Engenharia, Instituto Politécnico do Porto, Rua Dr António Bernardino de Almeida 431, 4200-072, Porto, Portugal.
authors.forename: Virgínia C
authors.initials: VC
authors.lastname: Fernandes
authors.forename: Diogo
authors.initials: D
authors.lastname: Pestana
authors.forename: Rosário
authors.initials: R
authors.lastname: Monteiro
authors.forename: Gil
authors.initials: G
authors.lastname: Faria
authors.forename: Manuela
authors.initials: M
authors.lastname: Meireles
authors.forename: Luísa
authors.initials: L
authors.lastname: Correia-Sá
authors.forename: Diana
authors.initials: D
authors.lastname: Teixeira
authors.forename: Ana
authors.initials: A
authors.lastname: Faria
authors.forename: Conceição
authors.initials: C
authors.lastname: Calhau
authors.forename: Valentina F
authors.initials: VF
authors.lastname: Domingues
authors.forename: Cristina
authors.initials: C
authors.lastname: Delerue-Matos
mesh_terms: D000273:Adipose Tissue / Q000737:chemistry*; D000537:Aluminum Oxide / Q000737:chemistry; D002849:Chromatography, Gas / Q000379:methods*; D006801:Humans; D006843:Hydrocarbons, Chlorinated / Q000032:analysis*; D057230:Limit of Detection; D010573:Pesticide Residues / Q000032:analysis*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry
chemical_list: D006843:Hydrocarbons, Chlorinated; D010573:Pesticide Residues; D000537:Aluminum Oxide