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Hydroxytyrosol extraction method high in percent conversion and recovery percent

A technology with high conversion rate of hydroxytyrosol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as agglomeration of oleuropein, troublesome process, and incomplete hydroxytyrosol, and achieve The effect of simplifying the process, shortening the production cycle and increasing the yield

Active Publication Date: 2014-04-09
GUILIN NATURAL INGREDIENTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method obtains a higher conversion rate (more than 85%) in a short production cycle, the one-time addition of acid hydrolysis will make the medicinal solution prone to agglomeration during the hydrolysis process, resulting in the hydrolysis of oleuropein. The conversion to hydroxytyrosol is incomplete, and the usual conversion rate is 85-90%; and this method requires two resin column chromatography, and the process is more troublesome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Take 500kg of olive leaves as raw material, crush them, add 75% (v / v) equivalent to 6 times the weight of the raw material, extract at 80°C for 120 minutes, and squeeze out the liquid medicine; then add 75% (v / v) equivalent to 6 times the weight of the raw material %(v / v), extract at 80°C for 120min, squeeze out the medicinal solution, combine the medicinal solutions, and filter to obtain the olive leaf extract; concentrate the extract under reduced pressure to an extract that is 0.5 times the weight of the raw material;

[0019] After determination, the content of oleuropein (seroiridoid glucoside oleuropein) in the extract was 6.96%. The determination method is (the same below): HPLC, chromatographic conditions: chromatographic column (Kromasil100-5C18); mobile phase: acetonitrile: water = 25:75, UV detection wavelength: 285nm, column temperature: 27°C, flow rate: 1mL / min .

[0020] 2) Add concentrated hydrochloric acid equivalent to 1% of the weight of the extrac...

Embodiment 2

[0027] 1) Take 500kg of olive leaves as raw material, crush them, add 90% (v / v) equivalent to 10 times the weight of the raw material, extract 150mim at 80-85°C, squeeze out the liquid medicine; then add an amount equivalent to 6 times the weight of the raw material 90% (v / v), extract 90mim at 80-85°C, press out the medicinal liquid, combine the medicinal liquid, and filter to obtain the olive leaf extract; concentrate the extract to an extract that is 0.6 times the weight of the raw material;

[0028] After determination, the content of oleuropein (seroiridoid glucoside oleuropein) in the extract was 5.77%. The method for measuring is the same as in Example 1.

[0029] 2) Add concentrated hydrochloric acid equivalent to 2% of the weight of the extract to the obtained extract, heat up to 95°C and heat-preserve for 20 minutes to hydrolyze; cool the obtained hydrolyzate to normal temperature, then add concentrated hydrochloric acid equivalent to 8% of the weight of the extract, ...

Embodiment 3

[0036]1) Take 500kg of olive leaves as raw material, crush them, add 80% (v / v) equivalent to 8 times the weight of the raw material, extract 100mim at 85°C, and squeeze out the liquid medicine; then add 80% (v / v) equivalent to 6 times the weight of the raw material %(v / v), extract 90mim at 85°C, squeeze out the liquid medicine; then add 70% (v / v) equivalent to 5 times the weight of raw materials, extract 30mim at 85°C, squeeze out the liquid medicine, and combine the liquid medicine , filter to obtain the olive leaf extract; concentrate the extract to an extract of 0.55 times the weight of the raw material;

[0037] After determination, the content of oleuropein (seroiridoid glucoside oleuropein) in the extract was 6.33%. The method for measuring is the same as in Example 1.

[0038] 2) Add concentrated hydrochloric acid equivalent to 1.5% of the weight of the extract to the obtained extract, heat up to 85°C and heat-preserve for 25 minutes for hydrolysis; cool the obtained h...

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Abstract

The invention discloses a hydroxytyrosol extraction method high in percent conversion and recovery percent. The hydroxytyrosol extraction method comprises the following steps of: 1) obtaining an olive leaf extract and concentrating the extract; 2) adding concentrated hydrochloric acid accounting for 1-2% of the weight of the extract to the obtained extract, increasing the temperature to the range from 85 to 95 DEG C, and preserving heat for hydrolysis for 20-40min; cooling the obtained hydrolysate to the normal temperature and then adding the concentrated hydrochloric acid accounting for 4-8% of the weight of the extract, and hydrolyzing at the normal temperature for 100-150 min to obtain a secondary hydrolysate; 3) regulating the pH value of the secondary hydrolysate to the range from 6.0 to 6.5, extracting with ethyl acetate, recovering the solvent from the extract phase, and drying to obtain the hydroxytyrosol. The hydroxytyrosol extraction method has the advantages that the pattern of intermittent twice hydrolysis is adopted, so that the shortcoming of non-complete once hydrolysis in the prior art is overcome and the percent conversion of decomposing and converting oleuropein into the hydroxytyrosol is effectively increased to be above 98.5%, and in the mean time, the yield of the hydroxytyrosol is increased to be above 95%, and moreover, the process is simplified.

Description

technical field [0001] The invention relates to a method for extracting effective components in plants, in particular to a method for extracting hydroxytyrosol with high conversion rate and high recovery rate. Background technique [0002] The chemical name of hydroxytyrosol (Hydroxytyrosol) is 3,4-dihydroxyphenethyl alcohol, which is a polyphenolic substance with the molecular formula C 8 h 10 o 3 , The relative molecular weight is 154. [0003] Hydroxytyrosol has safe and excellent antioxidant capacity, antibacterial, anticancer, anti-inflammatory and other biological and pharmacological activities. It can promote bone development and prevent cardiovascular and cerebrovascular diseases. In terms of anti-oxidation: it can promote metabolism, promote wound healing, eliminate free radicals in the body, restore the health of human organs, prevent brain failure, delay aging, and maintain youthful vitality; it can also protect human retinal epithelial cells, prevent and treat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/11C07C37/70
CPCC07C37/004C07C39/11
Inventor 杨文国宋云飞李元元梁远盛蒋治舟赵军
Owner GUILIN NATURAL INGREDIENTS CORP
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