Solid-phase extraction versus solid-phase microextraction for the determination of chlorinated paraffins in water using gas chromatography–negative chemical ionisation mass spectrometry

2004 ◽  
Vol 1025 (2) ◽  
pp. 157-162 ◽  
Author(s):  
P Castells ◽  
F.J Santos ◽  
M.T Galceran
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Phase Extraction ◽  
Ionisation Mass Spectrometry ◽  
Chlorinated Paraffins ◽  
Chemical Ionisation ◽  
Ionisation Mass

scholarly journals Headspace Solid-Phase Microextraction Coupled to Comprehensive Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometry for the Determination of Short-Chain Chlorinated Paraffins in Water Samples

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Nan Zhan ◽  
Feng Guo ◽  
Shuai Zhu ◽  
Zhu Rao
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Water Samples ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Short Chain ◽  
Two Dimensional ◽  
Flight Mass Spectrometry ◽  
Chlorinated Paraffins

Short-chain chlorinated paraffins (SCCPs) are a new type of persistent organic pollutants. In this work, a simple and effective method involving headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS) was developed and optimized for the determination of trace SCCPs in water samples. The key parameters related to extraction and separation efficiency were systematically optimized. The SCCP congener groups were best resolved using an Rxi-5Sil MS (30 m × 0.25 mm × 0.25 µm) column followed by an Rxi-17Sil MS (1.0 m × 0.15 mm × 0.15 µm) column; the optimum extraction conditions were achieved with a 100 µm polydimethylsiloxane SPME fiber, when a 10 mL water sample added with 3.6 g sodium chloride was incubated for 15 min at 90°C and then extracted during 60 min at 90°C and desorption at 260°C for 2 min. The proposed method showed good linearity in the concentration range of 0.2–20.0 µg/L with the determination coefficient greater than 0.995. The detection and quantification limits ranged from 0.06 to 0.13 µg/L and 0.18 to 0.40 µg/L, respectively, which are sufficient to meet the regulatory detection limits as set by most environmental regulations. The accuracy and precision of the method was also good, where the recoveries ranged from 82.5 to 95.4%, and intra- and interday precision was within 7.2% and 14.5%, respectively. The optimized method has been applied to the determination of SCCPs in ten freshwater samples of three different types.

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