Citation: LIU He-Huan, LI Hui-Ru, ZHANG Wen-Bing, SHENG Guo-Ying, FU Jia-Mo, PENG Ping-An. Co-analysis of Dechlorane Plus and Related Compounds in Soil Sample by Gas Chromatography Coupled with Triple Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(3): 423-428. doi: 10.11895/j.issn.0253-3820.160656 shu

Co-analysis of Dechlorane Plus and Related Compounds in Soil Sample by Gas Chromatography Coupled with Triple Tandem Mass Spectrometry

1.
State Key Laboratory of Organic Geochemistry and Guangdong Key Laboratory of Environmental Protection and Resources Utilization, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China;
2.
University of Chinese Academy of Science, Beijing 100049, China

Received Date: 5 September 2016
Revised Date: 13 January 2017

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 41273002), the Earmarked Fund of the State Key Laboratory of Organic Geochemicstry (No. SKLOD2015A02), and the Science and Technology Project of Guangdong Province, China (No. 2014B030301060)

A co-analysis method of gas chromatography coupled to a triple quadrupole mass spectrometry (GC-MS/MS) was developed for the determination of 11 kinds of Dechlorane plus (DP) related compounds, including DPs, dechlorinated DPs and its structural analogs. This method was successfully applied to the analysis of DPs in field soil samples. After clean-up through a multi-layer silica/aluminum column, the soil sample concentrate was measured with the following instrumental parameters:electron impact ion source, select reaction monitoring mode, DB-5HT capillary column (15 m×0.25 mm i. d., 0.1 μm), and temperatures for injection port, transfer line and ion source were 260℃, 280℃ and 250℃, respectively. About 1 μL of sample was injected in splitless mode with helium at 1.5 mL/min as carrier gas. The results showed that the analyte standard curves demonstrated linearity of 4 or 5 magnitude ranges with the correlation coefficient varying between 0.9977 and 0.9999. The instrumental detection limits for these analytes were in the range of 0.005-0.100 pg, and the relative standard deviations (RSDs) for 5 parallel analyses at concentration level of 50 pg/μL were 1.1%-19.8%. With this method, the total concentrations of DP and related compounds in the field soil samples from a typical polluted site and its surrounding area changed between 0.275 and 681 ng/g dw (dry weight) with a detection rate of 100%, and the concentrations for individual analyte varied from n.d. to 537 ng/g dw with anti-DP and syn-DP as the dominant pollutants. The mean recoveries of the two surrogate standards in all samples were 55.0%-103.0% and 83.4%-107.0%, respectively, and the mean recoveries and RSDs of all analytes in blank and matrix samples were 53.9%-117.0% and 6.0%-19.1%, respectively.
- Dechlorane plus,
- Gass chromatography-tnadem mass spectrometry,
- Soil,
- Halogenated flame retardant,
- Pesistent organic pollutants
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沈阳化工大学材料科学与工程学院沈阳 110142