Method and apparatus for the preparation of hydroxytyrosol-containing extracts from olive and olive oil extraction solid-containing residues
A technology of olive oil and olive pomace, applied in chemical instruments and methods, preparation of organic compounds, pressure vessels used in chemical processes, etc., can solve the difficulties of purification steps, increased degradation of hydroxytyrosol, and difficulty in removing harmful products, etc. question
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Embodiment 1
[0080] Extraction of hydroxytyrosol from olive waste (orujillo), purification of the aqueous phase
[0081] A 250 g sample of dried olive waste orujillo was mixed with 838 ml demineralized water and 16.7 g sulfuric acid (98%). The resulting mixture was kept in an autoclave at 121 °C for 30 minutes. Then, the aqueous phase was separated from the solid residue by filtration on a filter. The solid phase remaining on the filter was washed with 310 ml of demineralized water, the water from this washing operation being collected together with the previously recovered aqueous phase. Then about 860ml of the aqueous phase was centrifuged and refined to remove solid particles passing through the filter. After removal of the solids, 835 ml of crude aqueous extract was obtained containing 1.41 g of hydroxytyrosol with a HPLC purity of 47.5%.
Embodiment 2
[0083] Ion Exchange Hydroxytyrosol Purification
[0084] A 835 ml sample of the crude aqueous extract obtained according to Example 1 containing 1.41 g of hydroxytyrosol was loaded onto a column comprising an ion exchange resin of the anionic type previously activated by the acetate cycle. For example, Diaion WA10 can be used. The liquid phase recovered at the end of the column did not contain any hydroxytyrosol, and instead the column was continuously eluted with demineralized water until at least 90% of the initial charge of hydroxytyrosol was recovered. The eluate phase contained about 1.27 g of hydroxytyrosol with an HPLC purity of about 80.85%.
Embodiment 3
[0086] Ion exchange and adsorption of hydroxytyrosol purification
[0087] A 835 ml sample of the crude aqueous extract obtained according to Example 1 containing 1.41 g of hydroxytyrosol was loaded onto a column comprising an ion exchange resin of the anionic type previously activated by the acetate cycle. For example, IRA-67 can be used. The liquid phase recovered at the end of the column did not contain any hydroxytyrosol, and instead the column was continuously eluted with demineralized water until at least 90% of the initial charge of hydroxytyrosol was recovered.
[0088] The eluate phase from the first column is loaded onto the column containing the adsorptive resin. For example, resin XAD-1180 can be used. The liquid phase recovered at the end of the column does not contain any hydroxytyrosol. The hydroxytyrosol was then eluted from the resin with demineralized water until at least 90% of the initial charge of hydroxytyrosol was recovered. The eluate phase contai...
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