Solid phase microextraction coupled with comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry for high-resolution metabolite profiling in apples: Implementation of structured separations for optimization of sample preparation procedure in complex samples

2012 ◽  
Vol 1251 ◽  
pp. 208-218 ◽  
Author(s):  
Sanja Risticevic ◽  
Jennifer R. DeEll ◽  
Janusz Pawliszyn
2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Nan Zhan ◽  
Feng Guo ◽  
Shuai Zhu ◽  
Zhu Rao

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.


2016 ◽  
Vol 8 (22) ◽  
pp. 4509-4520 ◽  
Author(s):  
Anna Maria Sulej-Suchomska ◽  
Żaneta Polkowska ◽  
Tomasz Chmiel ◽  
Tomasz Marcin Dymerski ◽  
Zenon Józef Kokot ◽  
...  

Analysis of a new type of environmental sample – airport stormwater, a new analytical protocol (SPME/GC × GC-TOFMS) for tracking the environmental fate of PAHs.


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