Citation: ZHAN Nan, ZHU Shuai, GUO Feng, TIAN Qin, RAO Zhu. Determination of Short-Chain Chlorinated Paraffins in Water by Headspace Solid Phase Micro-extraction and Comprehensive Two-dimensional Gas Chromatography Time-of-Flight Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(12): 2004-2010. doi: 10.11895/j.issn.0253-3820.181309 shu

Determination of Short-Chain Chlorinated Paraffins in Water by Headspace Solid Phase Micro-extraction and Comprehensive Two-dimensional Gas Chromatography Time-of-Flight Mass Spectrometry

National Research Center for Geoanalysis, The Key Laboratory of Eco-geochemistry, Ministry of Nature Resources, Beijing 100037, China

Received Date: 9 May 2018
Revised Date: 21 September 2018

Fund Project: This work was supported by the National Research Center for Geoanalysis (No. CSJ2017012) and the China Geological Survey Programme (No. DD20189627) and the National natural Science Foundation of China(No. 21607033).

Short-chain chlorinated paraffins (SCCPs) are a new kind of persistent organic pollutant. Accurate analysis of SCCPs in water is important for good understanding of their pollution level, spatial distribution and environmental behavior in water environment. In this study, a simple, sensitive, and environmentally friendly method for the determination of trace SCCPs in water samples has been established based on headspace solid phase micro-extraction (HS-SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF-MS). The key parameters of HS-SPME were systematically optimized including fiber type, extraction temperature, extraction time, ionic strength, etc. Under the optimum extraction conditions, the calibration curves showed a good linearity (R² ≥ 0.999) in the concentration range of 0.2-20.0 μg/L. The detection limits of this method were 0.06-0.13 μg/L. The accuracy of the method was evaluated by calculating the recovery at 10 μg/L, resulting in good recovery values between 80.9% and 95.4%. The method precision was also satisfactory, with the RSD values less than 7.1% and 14.0% for intra-day and inter-day tests, respectively. Finally, the proposed method was applied to detection of SCCPs in real water samples of leather processing area in Hebei Province. In conclusion, the main advantages of the proposed method are the small sample volume, solvent-free extraction, automated online operation, and meeting the requirement of quality detection on SCCPs in water as set by most environmental regulations, thus we believe that this method is a good choice for the detection of SCCPs in water samples.
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