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Determination of PCBs in Aquatic Products by Dispersive Solid Phase Extraction-Gas Chromatography

HU Liyuan, DENG Jiyu, LIAO Hejing, SUN Gaoying, LIANG Dongjun, LIU Ruifang   

  1. 1. Dongxing Entry-Exit Inspection and Quarantine Bureau, Dongxing 538100, China;
    2. Dongxing City Aquatic Animal Husbandry and Veterinary, Dongxing 538100, China
  • Online:2016-07-25 Published:2016-07-26

Abstract:

This paper establishes a method for the batch analysis of seven polychlorinated biphenyls (PCBs) residues in
aquatic products by gas chromatography. The sample was extracted by ultrasonic assistance, and the extract was then
sulfonated with concentrated sulfuric acid before purification by dispersive solid-phase extraction (d-SPE). The efficiencies
of extraction and separation of PCBs were examined under different conditions and matrix interferences from aquatic
products were taken into account as well. Seven PCBs were detected by gas chromatography with electron capture detector
and quantitated using an internal standard calibration method. The results showed that the calibration curves of seven PCBs
had a good linearity within the concentration range of 0.005–0.2 μg/mL with correlation coefficient of 0.999 86–0.999 97.
The recoveries at spiked concentration levels of 2–100 μg/kg were 80.4%–118.0%, with relative standard deviations between
1.9% and 7.3%. The limit of detection (RSN = 3) was 0.4–0.8 μg/kg, and the practical quantification limit (RSN = 10) was
1.3–2.7 μg/kg. The method was characterized by simple operation, rapid detection and good reproducibility, and was suitable
for the batch analysis of PCBs residues in aquatic products.

Key words: ultrasonic extraction, dispersive solid-phase extraction, aquatic products, polychlorinated biphenyls (PCBs), matrix effect

CLC Number: