Optimisation of stir bar sorptive extraction applied to the determination of volatile compounds in vinegars
Stir bar sorptive extraction (SBSE) was evaluated for analysing volatile compounds in vinegar. The extraction and desorption analytical conditions have been optimised using a two-level factorial design expanded further to a central composite design. This chemometric tool is very appropriate in scree...
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Veröffentlicht in: | Journal of Chromatography A 2006-02, Vol.1104 (1), p.47-53 |
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Sprache: | eng |
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Zusammenfassung: | Stir bar sorptive extraction (SBSE) was evaluated for analysing volatile compounds in vinegar. The extraction and desorption analytical conditions have been optimised using a two-level factorial design expanded further to a central composite design. This chemometric tool is very appropriate in screening experiments where the aim is to investigate several possibly influential and/or interacting factors. For the extraction step, the optimum analytical conditions were: sample volume 25
ml without dilution, sampling time 120
min, NaCl content 5.85
g, and stirring speed 1250
rpm. For the desorption step, the optimised analytical conditions were: desorption temperature 300
°C, cryofocusing temperature −140
°C, flow of helium 75
ml
min
−1, and desorption time 10
min. The SBSE procedure developed shows detection limits, and linear ranges adequate for analysing this type of compounds. The repeatability values obtained were lower than 10%.
SBSE is a very simple, solvent-free, fast technique with better sensitivities, in general, than SPME. However, a disadvantage of this technique is that, up to now, the stir bar offers a limited enrichment capability for polar compounds because is only available with PDMS coating. |
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ISSN: | 0021-9673 |
DOI: | 10.1016/j.chroma.2005.12.006 |