Optimization of headspace solid-phase microextraction by means of an experimental design for the determination of methyl tert.-butyl ether in water by gas chromatography–flame ionization detection

2002 ◽  
Vol 963 (1-2) ◽  
pp. 259-264 ◽  
Author(s):  
Julien Dron ◽  
Rosa Garcia ◽  
Esmeralda Millán
2003 ◽  
Vol 86 (3) ◽  
pp. 461-466
Author(s):  
Jiemin Liu ◽  
Qunfang Zhou ◽  
Guibin Jiang ◽  
Jingfu Liu ◽  
Jiyan Liu ◽  
...  

Abstract A method based on headspace solid-phase microextraction and cryogenic gas chromatography with flame ionization detection was developed for the determination of volatile residual solvents in traditional Chinese medicines. A laboratory-made cryogenic chromatographic system was used for the separation of 15 kinds of residual solvents. During the analysis, a 65 μm PDMS/DVB fiber was used to extract the residual solvents, the extraction time was controlled at 0°C for 15 min, and the NaCl content of the sample was maintained at 30%. The limits of detection ranged from 0.08 (for octane) to 5000 μg/L (for ethanol), and the relative standard deviations were <8%. The recoveries from spiked samples ranged from 88 to 112%. Trace levels of residual solvents in several traditional Chinese medicines were effectively identified and quantified.


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