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J Chromatogr B Biomed Sci Appl. 2001 Jul 5;758(1):123-8.

Determination of acrolein by headspace solid-phase microextraction gas chromatography and mass spectrometry.

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  • 1Department of Pediatrics, Hiroshima University Faculty of Medicine, Japan.


We developed a headspace solid-phase microextraction (headspace SPME) method to measure acrolein in human urine. This new technique resolves some problems with the headspace gas chromatography and mass spectrometry (GC-MS) method which we developed previously. With the original method, a column and a filament were damaged by the injection of air. A 0.5-ml urine (or phosphate-buffered saline) sample in a glass vial containing propionaldehyde as an internal standard was heated for 5 min. The SPME fiber (65 microm carbonwax-divinylbenzene fiber) was exposed to the headspace and then inserted into a GC-MS instrument in which a DB-WAX capillary column (30 m x 0.32 mm, film thickness 0.5 degrees m) was installed. The total analysis time was 15 min. The inter-assay and intra-assay coefficients of variation were 10.07 and 5.79%, respectively. The calibration curve demonstrated good linearity throughout concentrations ranging from 1 to 10,000 nM. The headspace SPME method exhibits high sensitivity and requires a short analysis time as well as the previous method. We conclude that this method is useful to measure urinary acrolein.

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