An experimental test was conducted to obtain a rapid and complete extraction of polyphenols, optimizing the system in terms of:
The chemical analyzes are aimed at measuring the yield in total polyphenols, quite easy to identify, of great interest for pharmaceutical and nutriceutical applications, comparable with many literature data.
There is no mixing for ultrasonic extraction, as a very compact sonication cell is used.
The EW20S reactor consists of a main body ending with a 'barbell horn' type sonotrode and a compact flow cell, with a volume of approximately 100mL.
As regards the reference test (traditional maceration), the vegetable was immersed in the solvent at about 25 ° C for 48h.
Given the possibility of high specific powers involved, an external cooling system (ice) of the reactor was provided and the temperature rise was measured during the test, so as not to exceed 35 ° C for the vegetable mixture / solvent.
Main parameters for the optimized test:
Vegetal : THYME dry: density 0.21 g / l, 2 / 3mm, herbal tea cut
pre-treatment of veg.: 10 minutes of pre-immersion in water to soak the vegetables
solvent: H2O (60%) / EtOH (40%)
Vegetable / solvent dilution: 1/30
Power: 130W
temperature rise: about 15 ° C
Process type: BATCH, without mixing, with external cooling
reaction cell volume: 100mL
sonication time: 15min.
Results of chemical analysis
The results of the chemical analyzes on the extracts of the most significant tests follow.
The first set of analysis on the extraction tests was conducted with HPLC at a wavelength of 280 nm (characteristic for this class of compounds). In the figure relating to HPLC, the reference maceration test at room temperature is N 1, while the test optimized with ultrasound is N 11.
The trend of the graphs (quantity and height of the peaks) highlights the efficiency of ultrasound to extract various types of polyphenols in a few minutes (among these, various antioxidants: flavonoids known as proanthocyanidins, leucoanthocyanidins, piconogenols, tannins, etc., see following table).
After the first set of tests, the standard maceration and optimized US extractions were repeated and LC-MS (-) analyzes of the corresponding samples were performed. The relative chromatograms are almost identical (see figure: maceration N 17, ultrasound N 19), highlighting the total extraction capacity of the ultrasounds in reduced times. Very interesting is the analysis of the main polyphenols present in the extracts, listed in the table.
The analysis of the samples were carried out by the Institute of Biomolecular Chemistry of the C.N.R. of Padua, in the days immediately following that of the tests..
Conclusions
The results show an equivalent or greater extraction of polyphenols for the ultrasound test, compared to the extraction by traditional maceration.
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