Min Thai

CHE 158
Homework 9 Problem 3: Optimizing the selection of a reaction
Effects of extraction time, temperature and solvent on concentration and antioxidant
activity of grape marc phenolics
Giorgia Spigno, Lorenza Tramelli, Dante Marco De Faveri
Effects of extraction time, temperature and solvent on concentration and antioxidant
activity of grape marc phenolics by Giorgia Spigno, Lorenza Tramelli, Dante Marco De
Faveri describes the optimization in extracting total phenols (including: tannins,
anthocyanin, cinnamic acids, flavonols) from grapes. The selectivity and extraction were
improved by lowering the operating temperature, retention time of the grapes, and the
addition of water into the solvent base. Past experiments from other research facilities
were compared in regards to the extraction process of phenols in wine making.
Optimization parameters in the past experiments include: water content in ethanol, the
design of reactor, crushing of the marc grape, adding different compounds (acetone,
ethlacetate, methanol) to the solvent, varying solvent to solid ratio, and degreasing of the
pre-treatment.
Barbera red grapes, from Italy, were dried and milled to begin the extraction of phenols.
The range of parameters varied as listed below:
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Temperature of the experiment varied from 45 C and 60C. No intermediate

temperatures were used.

Retention time of the grapes varied from 1 hour, 3 hour, 5 hour, 7 hour, 9 hour, 15

hour, 20 hour and 24 hour.

Using the solution from trial of temperature of 60C and 5 hour, different volumes
were added to this particular solution. Volumes range from 10%, 20%, 30%,

40%, 50% and 60%

Freeze Dried vs. Liquid Extracts were also compared

In order to determine the amount of phenols extracted from the solution, the FolinCiocalteu method and absorption at 280 nm were used to determine the following results.

Temperature - the maximum yield is at 45 C instead of 60 C, however, it is cheaper to

work at 60C, as the retention time is shorter. Higher operation cost is to be considered
with the higher retention time, therefore 60C is more economical. Although the greater
temperature would generate a higher energy cost, the amount of operation time required
at 45C about 20 hour compared to 60C for about less than 8 hours is substantial. It is also
important to take in the extraction rate and to consider the importance of streamlining
manufacturing process in a plant.

Retention Time - Should not be greater than 20 hours. After 20 hours, the extraction rate
of the phenols decrease substantially. From Figure 1, it is apparent that the %yield of the
phenols increase dramatically within the first 10 hours, and gradually from 10 -20 hours,
finally decreasing by approximately 1 -3% after the 20 hours.
Addition of water - increases the extraction of the phenols, however, the volume added
can also affect the extraction of other undesired compounds. However, having the
presence of these undesired products would then lower the concentration of extracted
phenols. Therefore, it is important to monitor the volume of water added to the solvent
base.