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Process and apparatus for the production of hydroxytyrosol containing extract from olives and solids containing residues of olive oil extraction

A technology of hydroxytyrosol and olive oil, applied in chemical instruments and methods, preparation of organic compounds, pressure vessels used in chemical processes, etc., can solve problems such as increased degradation of hydroxytyrosol, high oleuropein content, and harsh conditions , to achieve a good yield

Active Publication Date: 2010-01-20
欧罗麦德股份公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first drawback is the increased degradation of hydroxytyrosol under neutral and alkaline conditions, the appearance of harmful products that are difficult to remove, and, due to the fact that no acid hydrolysis is performed, the oleuropein content will still be high
Second, the achievable concentration factors are poor, so the maximum permissible concentration of hydroxytyrosol according to Example 1 (see Table 1) is in the range of 1.2-1.6 g / L
[0017] In summary, the techniques mentioned above are either too long, or too complex, or too harsh, or have all of the above disadvantages; this results in residual oleuropein, i.e. unhydrolyzed, and / or hydrolyzed by-products such as The amount of hydroxymethylfurfural was high enough to make subsequent purification steps difficult

Method used

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  • Process and apparatus for the production of hydroxytyrosol containing extract from olives and solids containing residues of olive oil extraction
  • Process and apparatus for the production of hydroxytyrosol containing extract from olives and solids containing residues of olive oil extraction
  • Process and apparatus for the production of hydroxytyrosol containing extract from olives and solids containing residues of olive oil extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Extraction of hydroxytyrosol from olive waste (orujillo), purification of the aqueous phase

[0073] A 250 g sample of the dried olive waste oruillo 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. The aqueous phase was then 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, and the water from this washing operation was collected together with the previously recovered aqueous phase. About 860 ml of the aqueous phase was then purified by centrifugation to remove solid particulates that passed through the filter. After removal of the solids, 835 ml of crude water extract were obtained containing 1.41 g of hydroxytyrosol with HPLC purity of 47.5%.

Embodiment 2

[0075] Ion Exchange Hydroxytyrosol Purification

[0076] 835 ml of a sample of the crude aqueous extract obtained according to Example 1, containing 1.41 g of hydroxytyrosol, were loaded onto a column containing an anionic ion exchange resin previously activated by acetate cycling. 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 approximately 1.27 g of hydroxytyrosol with an HPLC purity of approximately 80.85%.

Embodiment 3

[0078] Ion exchange and adsorption of hydroxytyrosol purification

[0079] 835 ml of a sample of the crude aqueous extract obtained according to Example 1, containing 1.41 g of hydroxytyrosol, were loaded onto a column containing an anionic ion exchange resin previously activated by acetate cycling. 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.

[0080] The eluate phase from the first column is loaded onto a column containing an adsorbent resin. For example, resin XAD-1180 can be used. The liquid phase recovered at the end of the column did not contain any hydroxytyrosol. The hydroxytyrosol is then eluted from the resin with demineralized water until at least 90% of the initial charge of hydroxytyrosol is recovered. The eluate phase contained approximate...

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Abstract

The invention discloses a method for producing hydroxytyrosol from olives and solids containing residues of olive oil extraction, which comprises: performing acid hydrolysis under the temperature between 110 and 140 degrees centigrade and the pH value between 1.0 to 6.0; purifying the obtained solution on a column containing acid activated anion exchange resin and a column containing sorptive non-ionic resin; and eluting the two columns by water to recover the hydroxytyrosol.

Description

field of invention [0001] The present invention relates to a method and a device for the preparation of an extract comprising hydroxytyrosol from olives and / or olive residue comprising solids after extraction of olive oil. More particularly, the present invention relates to the preparation of extracts comprising hydroxytyrosol to be used as a source of hydroxytyrosol in the food, pharmaceutical and cosmetic industries. Background of the invention [0002] It is now well known that olives contain many bioactive compounds, especially polyphenols; among these polyphenols, hydroxytyrosol is of outstanding biological interest due to its antioxidant, antimicrobial and free radical scavenging activities. [0003] Hydroxytyrosol has the formula: [0004] [0005] The preparation of hydroxytyrosol from olive residue after oil extraction was and is actively researched; efficient extraction methods may be of particular interest, not least because of the major amounts of hydroxytyro...

Claims

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Application Information

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IPC IPC(8): C07C37/01C07C39/11B01J3/04
CPCC07C37/004B01J2219/00006C07C37/68C07C37/70B01J2219/00177C07C37/82
Inventor J·A·洛佩斯马斯S·A·斯特雷登贝格尔M·佩尼亚尔韦尔梅利亚多P·马丁内斯奥尔蒂斯
Owner 欧罗麦德股份公司
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