DESENVOLVIMENTO E CARACTERIZAÇÃO FÍSICO ... - UFSM

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sum of areas and sum of peaks were corresponding to the mixed-polymer coating fiber,
DVB/CAR/PDMS (50/30 µm × 20 mm). CAR/PDMS fiber, which represents another mixedpolymer
coating, extracted 123 volatile compounds and the sum of peak areas of these
compounds was lower than DVB/CAR/PDMS value. Mixed-polymer coating fibers presented
a high retention capacity due to the mutually potentiating effect of adsorption and distribution
to the stationary phase 15,31 . The extraction with PDMS fiber, a non-polar coating, showed the
lowest results for the evaluated parameters. Although DVB/Car/PDMS has the greatest surface
area (fiber with 20 mm), which probably had an improvement in the extraction efficiency.
Additionally, the affinity of the fiber coating for an analyte is the most important factor
in SPME according to Kataoka 15 . As will be shown further, the predominant compounds in jelly
palm wine are esters followed by alcohols. Furthermore, previous studies showed that the
combination of the three stationary phases, DVB/CAR/PDMS, is the most appropriate due to
its extraction ability over an expanded range of compounds, including analyses of volatile
compounds from wine samples 32,33,34 . Based on these results, further optimization of the
method, including the SPME sampling time, temperature and salt addiction were carried out
with the DVB/CAR/PDMS fiber. The results of the effect of different sampling temperature
and time (Table 3) showed that the optimal condition for these parameters were, 35 °C for
extraction temperature and 45 min for extraction time, always preceded of 5 min of equilibrium.
Raising the temperature from 25 °C to 35 °C a significant increase of total area was observed.
However, when the temperature reach 45 ºC no significant difference was observed compared
to 35 °C (p > 0.05), at this point, the total area showed a slight decrease, which means that, the
compounds adsorbed on the fiber begun to perform the reverse process of desorption.
According to Pellati 35 the increase in sampling temperature increased the headspace
concentration of the volatile compounds, favoring the extraction. However, SPME involves an
exothermic process and the extraction of compounds decreases as the temperature increases 33 .
Though temperatures of 35 and 45 ºC were not statistically different, 35 °C was the chosen one
since 45 ºC could lead to a sensory decharacterization of the jelly palm wine. Time extraction
increases de total area with significant difference between 30 and 45 min (p > 0.05).
However, between 45 and 60 min no significant difference was showed. These results
are demonstrating that, extraction time influences the equilibrium between the analytes
concentration in the aqueous phase and in the polymeric phase of the fiber 29 . Once the
equilibrium has been reached, the analyte concentration in the fiber decreases. The same
behavior has been observed in other samples such as, oregano and grape 36,16 . The results found
for the salt addiction were the same found for other authors in similar matrices 7,37,38 and confirm