Citation: HU Hong-Mei, GUO Yuan-Ming, HAO Qing, SUN Xiu-Mei, JIN Yan-Jian, ZHONG Zhi, LI Tie-Jun. Determination of Polychlorinated Biphenyls in Soil or Sediment by Gas Chromatography-Electron Capture Detection Combined with Ultrasonic Extraction and Dispersive Solid Phase Extraction Cleanup[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(1): 88-94. doi: 10.11895/j.issn.0253-3820.150544 shu

Determination of Polychlorinated Biphenyls in Soil or Sediment by Gas Chromatography-Electron Capture Detection Combined with Ultrasonic Extraction and Dispersive Solid Phase Extraction Cleanup

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Marine Fishery Institute of Zhejiang Province, Key Laboratory of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang Province, Zhoushan 316021, China

Corresponding author: GUO Yuan-Ming,
Received Date: 7 July 2015
Available Online: 16 November 2015
Fund Project: 本文系国家自然科学基金(No.21407127) (No.21407127)浙江省自然科学基金(Nos.LQ13C200004,LQ14B070002)资助项目 (Nos.LQ13C200004,LQ14B070002)

A simple, rapid, efficient, sensitive and low matrix interference method for the determination of 7 specified polychlorinated biphenyls (PCBs) in soil or sediment samples using gas chromatography-electron capture detection (GC-ECD) combined with ultrasonic extraction and dispersive solid phase extraction (DSPE) cleanup was described. The step of concentrated sulfuric acid purification could be chosen flexibly according to the color of the extract, and the kinds and amounts of adsorbent were optimized. If the extract was basically colorless transparent, only 150 mg of primary secondary amine (PSA) was used for DSPE cleanup (one-step purification process), otherwise it needed a purification for the extract by concentrated sulfuric acid and 100 mg of PSA for the DSPE cleanup (two-step purification process). The whole DSPE cleanup process only needed less than 5 min, which significantly shortened the sample pretreatment time. The linearity of the method ranged from 1.25 μg/L to 100 μg/L for 7 PCBs, with correlation coefficients ranging from 0.9990 to 0.9999. The detection limits for 7 PCBs were 0.02-0.03 μg/kg. The recoveries of spiked PCBs at different concentration levels in samples with two-step purification process (concentrated sulfuric acid purification and DSPE cleanup) and one-step purification process (only DSPE cleanup) were 72%-107%, and 88%-115%, respectively, with relative standard deviations (RSDs) of 3.5%-5.8%, and 3.7%-6.9% (n=5), respectively. The performance of the proposed method was compared with national standard methods on the real water samples (i.e., soil samples in certain vegetable patch of Zhujiajian, Zhoushan, sediment samples in waters of Daiquyang, Zhoushan, etc.) and comparable efficiencies were obtained. It was concluded that this method could be successfully applied for the determination of PCBs in soil or sediment with good accuracy and precision.
- Ultrasonic extraction,
- Dispersive solid phase extraction,
- Gas chromatography-electron capture detection,
- Polychlorinated biphenyls,
- Soil,
- Sediment
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