Optimization of thin film-microextraction (TF-SPME) method in order to determine musts volatile compounds
Analytica Chimica Acta(2022)
摘要
It is well known that grape aromatic composition is directly correlated to the final wine quality. To determine this composition, a previous stage of selective extraction is necessary, since the aromatic compounds are found in very low concentrations in the grapes. Therefore, in this work, the thin film microextraction technique (TF-SPME) was optimized, for first time, with the aim to analyze the volatile composition of the grape musts. The results obtained with the two commercially available absorbent materials for TF-SPME, polydimethylsiloxane/carboxene (PDMS/CAR) and PDMS/divinylbenzene (PDMS/DVB), were optimized and compared. To carry out the optimization, a randomized factorial design was performed combining the following factors and levels: extraction mode (headspace (HS), or direct immersion (DI)), stirring speed (500 and 1000 rpm), extraction time (1, 3 and 6 h), and extraction temperature (20, 40 and 60 °C). After performing a principal component analysis (PCA) and an analysis of variance (ANOVA) multifactorial, it was concluded that the best conditions for TF-SPME with PDMS/CAR were: direct immersion (DI), 500 rpm, 6 h, and 20 °C, while for TF-SPME with PDMS/DVB no conditions were found that maximized the extraction of most compounds, therefore compromise conditions were chosen: headspace (HS), 500 rpm, 6 h, and 40 °C. Finally, the comparison between the results obtained with both absorbents indicated that the absorbent that extracted better the volatile compounds from the musts with the TF-SPME technique, was PDMS/CAR, under the conditions: direct immersion (DI), 500 rpm, 6 h, and 20 °C.
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关键词
TF-SPME,Optimization,Extraction,Comparison,Grape aroma,PDMS/CAR and PDMS/DVB absorbents
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