title: Optimisation of matrix solid-phase dispersion for the determination of Dechlorane compounds in marketed fish.
abstract: A method for the determination of chlorinated flame retardants: Dechlorane Plus, Dechlorane (Dec) 602, Dec 603 and Dec 604, in marketed fish is described. The method involves the use of matrix solid-phase dispersion (MSPD) prior to their determination by gas chromatography-electron-capture negative-ion chemical-ionisation mass spectrometry (GC-ECNICI-MS). Parameters that affect the extraction efficiency of the target analytes from fish samples were optimised using a Box-Behnken design method. MSPD integrated the extraction and clean-up procedures into a single step, which provides the benefits of being simple and convenient. The optimal extraction conditions involved dispersing a freeze-dried fish (1-g) in 2-g of silica gel, and packed with 1-g of Florisil, and then the target analytes were eluted with 20 mL of n-hexane. The limits of quantification were 9-15 pg/g-lipid weight. Preliminary results showed that the total concentrations of the target analytes ranged from 0.15 to 1.3 ng/g-lipid weight.
authors.affiliation: Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
authors.forename: Chien-Liang
authors.initials: CL
authors.lastname: Chen
authors.affiliation: Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
authors.forename: Dung-Ying
authors.initials: DY
authors.lastname: Tsai
authors.affiliation: Department of Chemistry, National Central University, Chung-Li 320, Taiwan. Electronic address: wanghsiending@gmail.com.
authors.forename: Wang-Hsien
authors.initials: WH
authors.lastname: Ding
mesh_terms: D000818:Animals; D005399:Fishes; D005411:Flame Retardants / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006843:Hydrocarbons, Chlorinated / Q000032:analysis / Q000737:chemistry; D015394:Molecular Structure; D011083:Polycyclic Compounds / Q000032:analysis / Q000737:chemistry; D015203:Reproducibility of Results; D017747:Seafood / Q000032:analysis*; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D005411:Flame Retardants; D006843:Hydrocarbons, Chlorinated; D011083:Polycyclic Compounds; D014874:Water Pollutants, Chemical; C556733:dechlorane 602; C556736:dechlorane 603; C556738:dechlorane 604; C526360:dechlorane plus
keywords: Dechlorane compounds; Fish sample analysis; GC–ECNICI-MS; Matrix solid-phase dispersion