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Supercritical CO2 extraction of grape-kernel oil and method for extracting oligoprotoanthocyanidin by solvent process

A technology for oligomeric proanthocyanidins and grape seed oil, which is applied in the fields of supercritical CO2 extraction of grape seed oil and solvent extraction of oligomeric proanthocyanidins, can solve problems such as unsatisfactory research results, and achieve pure naturalness and good thermal stability. and storage, the effect of no solvent residues

Inactive Publication Date: 2009-03-18
王芳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

French M.C Andry et al. used the polymerization method to form a protective film on the surface of proanthocyanidins and terephthaloyl chloride, and the research results were not very satisfactory.

Method used

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  • Supercritical CO2 extraction of grape-kernel oil and method for extracting oligoprotoanthocyanidin by solvent process

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Experimental program
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Effect test

Embodiment 1

[0026] In the experiment, the grape seed powder obtained after crushing and drying was used as raw material, and supercritical CO was used to 2 (SC-CO 2 ) extraction technology, the flow of the test device is as follows figure 1 shown. The supercritical extraction device is mainly composed of the following parts: CO 2 Gas cylinder 1, filtration and purification device 2, storage tank 3, cold box 4, flow plunger metering pump 5, check valve 6, mixer 7, preheater 8, extraction kettle 9, separator 10, etc.

[0027] Accurately weigh the grape seed powder with crushed particle size of 20 mesh, 40 mesh and 60 mesh respectively, put them in the extractor, and carry out dynamic extraction under the set extraction conditions. Supercritical CO with grape seed oil dissolved 2 After decompression and heating, it is separated from the grape seed oil. After the extraction is completed, the weight of the extract is accurately weighed, and the oil content in the grape seed powder is measur...

Embodiment 2

[0031] The extracts in the actual system will contain a certain amount of water, and the oil and fat are extracted using the carbon dioxide critical fluid. The water content in the material is an important factor affecting the extraction yield. Grape seeds with water content of 0.5%, 4.5% and 7.7% were selected for extraction such as image 3 , at a pressure of 30MPa and a temperature of 45°C, CO 2Under the extraction condition of flow rate of 10L / h, 40 mesh grape seed oil was collected after 90 minutes, and the yields of grape seed oil were 40%, 98.53% and 97.62% respectively, and there was white precipitate in the product when the water content was high Precipitation, and the pipeline freezes up. It can be seen that the water content cannot be too high or too low, and the extraction rate of grape seed oil is the highest when it is about 4.5%, and the quality is also the best.

Embodiment 3

[0033] Other conditions are constant, as the pressure situation increases, the oil rate also increases eventually, and the time used also decreases, such as Figure 4 , at 30MPa, the extraction rate reached 98.53% after 90 minutes, 60% and 82% at 20MPa and 25MPa, respectively, and then both reached the maximum after 30 minutes and 60 minutes. This is because as the pressure increases, the supercritical CO 2 As the density increases, its solvency also increases, which strengthens the relationship between grape seed oil and supercritical CO 2 The solvation improves the extraction efficiency and shortens the equilibrium time relatively. However, when the pressure is relatively high, the pigment content in the extract will increase and the color will deepen, which will have a certain impact on the quality of the product. Considering the practicability of production, it is better to choose the extraction pressure in the range of 25-30MPa.

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Abstract

The invention discloses a method for extracting grape-kernel oil by supercritical CO2 and oligo-raw anthocyanin by the solvent method, wherein the raw anthocyanin obtained is subjected to chromatographic separation and microencapsulation technical treatment, so as to obviously improve the purity and the thermal stability of the raw anthocyanin. The method guarantees the pure natural property of the product, has the characteristics of simpleness, convenience, quickness and easy operation, and can obtain higher efficiency. The method comprises the following steps: the grape-kernel oil is extracted by an extraction device, wherein the grinding degree of grape-kernel is between 40 and 60 meshes, the moisture content is between 3 and 7 percent, the flow rate of the CO2 is between 1 and 15 liters per hour, the pressure is between 30 and 50 MPa, the temperature is between 40 and 60 DEG C, and the separation pressure in a separator is between 5 and 10 MPa; a raw anthocyanin oligomer is extracted from grape-kernel dregs, wherein the grinding degree of the grape-kernel dregs is between 20 and 60 meshes, the concentration of ethanol is between 40 and 80 percent, the solid-liquid ratio is 1 to 8, the extraction temperature is between 40 and 60 DEG C, the concentration of acetic acid is between 0.1 and 2 percent, and the extraction time is between 1 and 2 hours, and extraction is repeatedly performed twice; and the raw anthocyanin is subjected to chromatographic separation, static and dynamic adsorption by macroporous absorbent resin, and elution twice by acetic ether and acetone, and then the oligo-raw anthocyanin with strong antioxidation and strong ability in eliminating free radicals is formed after combination.

Description

technical field [0001] The present invention relates to a kind of supercritical CO 2 The method for extracting grape seed oil and extracting proanthocyanidins by solvent method and the technical treatment of heat stability and storage of the obtained proanthocyanidins. Background technique [0002] Grape seeds are the leftovers of the winery, accounting for 5%-7% of the grain weight. Grape seeds contain 14%-17% oil, of which oleic acid content is as high as 68%-76%, and grape seed oil also contains a variety of fat-soluble vitamins. Grape seed extract mainly contains oligomeric proanthocyanidins, which are known for their high efficiency, low toxicity and high bioavailability. Proanthocyanidins have strong antioxidant capacity, and its antioxidant and free radical scavenging capacity in the body is 50 times that of vitamin E and 20 times that of vitamin C. [0003] The preparation methods of grape seed oil mainly include mechanical pressing, pre-pressing leaching, one-time...

Claims

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Application Information

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IPC IPC(8): C11B1/10C07D311/60C07D311/62
CPCY02P20/54
Inventor 王芳
Owner 王芳
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