title: Screening and determination of polycyclic aromatic hydrocarbons in seafoods using QuEChERS-based extraction and high-performance liquid chromatography with fluorescence detection.
abstract: A rapid, sensitive, and accurate method for the screening and determination of polycyclic aromatic hydrocarbons (PAHs) in edible seafood is described. The method uses quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction and HPLC with fluorescence detection (FLD). The method was developed and validated in response to the massive Deepwater Horizon oil spill in the Gulf of Mexico. Rapid and highly sensitive PAH screening methods are critical tools needed for oil spill response; they help to assess when seafood is safe for harvesting and consumption. Sample preparation involves SPE of edible seafood portions with acetonitrile, followed by the addition of salts to induce water partitioning. After centrifugation, a portion of the acetonitrile layer is filtered prior to analysis via HPLC-FLD. The chromatographic method uses a polymeric C18 stationary phase designed for PAH analysis with gradient elution, and it resolves 15 U.S. Environmental Protection Agency priority parent PAHs in fewer than 20 min. The procedure was validated in three laboratories for the parent PAHs using spike recovery experiments at PAH fortification levels ranging from 25 to 10 000 microg/kg in oysters, shrimp, crab, and finfish, with recoveries ranging from 78 to 99%. Additional validation was conducted for a series of alkylated homologs of naphthalene, dibenzothiophene, and phenanthrene, with recoveries ranging from 87 to 128%. Method accuracy was further assessed based on analysis of National Institute of Standards and Technology Standard Reference Material 1974b. The method provides method detection limits in the sub to low ppb (microg/kg) range, and practical LOQs in the low ppb (microg/kg) range for most of the PAH compounds studied.
authors.affiliation: Food and Drug Administration, Forensic Chemistry Center (FCC), 6751 Steger Dr, Cincinnati, OH 45237, USA. Samuel.gratz@fda.hhs.gov
authors.forename: Samuel R
authors.initials: SR
authors.lastname: Gratz
authors.forename: Laura A
authors.initials: LA
authors.lastname: Ciolino
authors.forename: Angela S
authors.initials: AS
authors.lastname: Mohrhaus
authors.forename: Bryan M
authors.initials: BM
authors.lastname: Gamble
authors.forename: Jill M
authors.initials: JM
authors.lastname: Gracie
authors.forename: David S
authors.initials: DS
authors.lastname: Jackson
authors.forename: John P
authors.initials: JP
authors.lastname: Roetting
authors.forename: Heather A
authors.initials: HA
authors.lastname: McCauley
authors.forename: Douglas T
authors.initials: DT
authors.lastname: Heitkemper
authors.forename: Fred L
authors.initials: FL
authors.lastname: Fricke
authors.forename: Walter J
authors.initials: WJ
authors.lastname: Krol
authors.forename: Terri L
authors.initials: TL
authors.lastname: Arsenault
authors.forename: Jason C
authors.initials: JC
authors.lastname: White
authors.forename: Michele M
authors.initials: MM
authors.lastname: Flottmeyer
authors.forename: Yoko S
authors.initials: YS
authors.lastname: Johnson
mesh_terms: D000478:Alkylation; D000818:Animals; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry; D007202:Indicators and Reagents; D057230:Limit of Detection; D059392:Petroleum Pollution; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis*; D012015:Reference Standards; D015203:Reproducibility of Results; D017747:Seafood / Q000032:analysis*; D012758:Shellfish; D013050:Spectrometry, Fluorescence; D014481:United States; D014484:United States Environmental Protection Agency
chemical_list: D007202:Indicators and Reagents; D011084:Polycyclic Aromatic Hydrocarbons