Obtaining Hydroxytyrosol from Olive Mill Waste Using Deep Eutectic Solvents and Then Supercritical CO 2
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ORIGINAL PAPER
Obtaining Hydroxytyrosol from Olive Mill Waste Using Deep Eutectic Solvents and Then Supercritical CO2 Andrea Plaza1,3 · Ximena Tapia1 · Camila Yañez1 · Fernanda Vilches2 · Oscar Candia1,3 · René Cabezas2 · Julio Romero2 Received: 6 March 2019 / Accepted: 24 September 2019 © Springer Nature B.V. 2019
Abstract The main objective of this study was to recover hydroxytyrosol from olive mill waste (olive leaves and a semi-solid waste with a 65–75% of humidity called alperujo). The recovery process involved solid–liquid extractions using two hydrophilic deep eutectic solvents (DESs), CIS-DES (a 1:1 mixture of choline chloride and citric acid) and Etagline (a 1:2 mixture of choline chloride and ethylene glycol). The results achieved using this non-conventional process was compared with the results achieved using conventional solid–liquid extraction processes using ethanol, methanol, and water. The extraction ratio (R) achieved using Etagline DES was 11.4 times higher than the R achieved using methanol. The hydroxytyrosol extraction efficiencies were higher when using the selected DESs than using methanol, under the same working conditions. On the other hand, with the use of DES it is possible to obtain similar extraction efficiencies to those obtained with organic solvents, but using 75% less extraction phase, when DESs were used instead of methanol. The DES extraction processes gave high re-extraction capacities when supercritical CO2 was used as a stripping phase. The highest pure hydroxytyrosol extraction efficiency, 80%, was achieved using Etagline and supercritical C O2 re-extraction at a pressure and temperature close to the critical values. The results suggest that DES is an efficient, safe, and sustainable alternative to methanol for extracting bioactive compounds from olive mill waste and that DES extraction combined with supercritical CO2 extraction can be classed as a green process. Graphic Abstract
DES
DES
DES
Extract
OMW DES
DES
OL
CO2
S/L Extraction Process Hydroxytyrosol DES: Deep Eutectic Solvents
Tyrosol OMW: Olive Mill Wastes
SCE
Oleuropein OL: Olive Leaves SCE: Supercritical extraction
Keywords Hydroxytyrosol recovery · Olive mill wastes · Deep eutectic solvent extraction · Supercritical fluid extraction · Green process
* Andrea Plaza [email protected] Extended author information available on the last page of the article
Abbreviations HT Hydroxytyrosol T Tyrosol OI Oleuropeine
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Vol.:(0123456789)
OMW Olive mill waste OL Olive leaves DESs Deep Eutectic Solvents CO2 Carbon dioxide EtOH Ethanol MetOH Methanol HPLC High performance liquid chromatography R Extraction ratio SCE Supercritical fluid extraction GAE Gallic acid equivalent w/w Refer to mass fraction v/v Referred to volume/volume percent DW Dry waste S/L Solid/liquid extraction process
Statement of Novelty Olive oil production hides one of the strongest antioxidants within its byproducts, Hydroxytyrosol (HT). Due to its hydrophilic nature, the concentration of this polyphenol is greater
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