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Multi-stir bar sorptive extraction for analysis of odor compounds in aqueous samples

Ochiai, Nobuo ; Sasamoto, Kikuo ; Ieda, Teruyo ; David, Frank ; Sandra, Pat

Journal of Chromatography A, 2013-11, Vol.1315, p.70-79 [Revista revisada por pares]

Amsterdam: Elsevier B.V

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  • Título:
    Multi-stir bar sorptive extraction for analysis of odor compounds in aqueous samples
  • Autor: Ochiai, Nobuo ; Sasamoto, Kikuo ; Ieda, Teruyo ; David, Frank ; Sandra, Pat
  • Materias: Analytical chemistry ; Bars ; Biological and medical sciences ; Chemistry ; Chromatographic methods and physical methods associated with chromatography ; Coating ; Coffee, tea and other stimulative beverage industries ; EG Silicone stir bar ; Enrichment ; Exact sciences and technology ; Extraction ; Food industries ; Fundamental and applied biological sciences. Psychology ; Gas chromatographic methods ; GC–MS ; Multi-SBSE (mSBSE) ; Odor analysis ; Odors ; PDMS stir bar ; Silicone resins ; Silicones ; Stirring ; Thermal desorption
  • Es parte de: Journal of Chromatography A, 2013-11, Vol.1315, p.70-79
  • Notas: ObjectType-Article-1
    SourceType-Scholarly Journals-1
    ObjectType-Feature-2
    content type line 23
  • Descripción: •We examine multi-stir bar sorptive extraction (mSBSE) and GC–MS for odor analysis.•A new sampling mode greatly improves performance of the EG Silicone stir bar.•The EG Silicone stir bar allows higher recovery of polar solutes in aqueous samples.•The method provides more uniform enrichment compared to conventional SBSE.•Analyses of odor compounds in roasted green tea are demonstrated. As reproducible coating of stir bars with more polar phases was found to be very difficult, a supporting grid was used in the development of an ethyleneglycol-modified Silicone (EG Silicone) coated stir bar. This new polar coating showed good performance for the extraction of polar solutes, but long term use also showed degradation of the coating due to friction while stirring. In order to address the lower robustness of the EG Silicone stir bar which has a much softer coating compared to a conventional polydimethylsiloxane (PDMS) stir bar, a novel SBSE procedure termed multi-SBSE (mSBSE) was developed. mSBSE consists of the robust PDMS stir bar stirring at the bottom of the vial and the EG Silicone stir bar attached on the inner side wall of the vial (a magnetic clip is used for the set-up). After extraction, the two stir bars are placed in a single glass desorption liner and are simultaneously thermally desorbed. The desorbed compounds were analyzed by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS). Compared to conventional SBSE, mSBSE provides more uniform enrichment of a wide range of odor compounds in aqueous sample since both stir bars can complement each other, while eliminating the damage of the EG Silicone phase during the extraction. The robustness of the EG Silicone stir bar was dramatically increased and more than 30 extraction and desorption cycles were possible without loss in performance. The recoveries for polar solutes such as 2-acetyl pyrrole (logKow: 0.55), benzyl alcohol (logKow: 1.08), guaiacol (logKow: 1.34), and indole (logKow: 2.05) were increased by a factor of about 2–7. The mSBSE–TD–GC–MS method showed good linearity (r2>0.9913) and high sensitivity (limit of detection: 0.011–0.071ngmL−1) for the test compounds spiked in water. The feasibility and benefit of the method was demonstrated with analysis of odor compounds in roasted green tea. The normalized areas obtained from mSBSE showed the best enrichment for most of the selected compounds compared to conventional SBSE using the PDMS stir bar or the EG Silicone stir bar. Fifteen compounds were determined in the range of 0.15–210ngmL−1 (RSD<14%, n=6).
  • Editor: Amsterdam: Elsevier B.V
  • Idioma: Inglés
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