Abstract: Objective: To establish a method for the extraction and determination of five volatile halogenerated hydrocarbons (VHHs) in edible oil by headspace solid-phase microextraction (HS-SPME) and gas chromatography-electron capture detector (GC-ECD). Methods: Samples were subjected to headspace extraction with 5 types of fiber (Supelco Inc.). Extraction efficiencies of different fibers were compared, and the effects of extraction temperature, extraction time, and solvent volume were investigated. The chromatographic separation was carried out on a capillary column equipped to a gas chromatography system with electron capture detector. Results: CAR/PDMS fiber of 75μm was the selected fiber. After pouring 9 mL of edible oil in a 15 mL vial, the extraction was conducted at the equilibrium temperature of 60 ℃ and extraction time of 30 min. The desorption of fiber was performed at 290 ℃ for 3 min. The detection limit of the established method ranged from 0.02 (tetrachloroethylene) to 1.4 ng/mL (trichloro ethane). The average recovery rate was in the range of 89%－105% with a relative standard derivation (RSD) of less than 8.5%. Conclusion: This method is simple, practical, and sensitive, which is suitable for the determination of VHHs in edible oil.

Key words: edible oil, headspace solid-phase microextraction, volatile halogenerated hydrocarbons, gas chromatography, hyphenated technology