Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling

A technology of camellia oil cake and boiling under reduced pressure, applied in chemical instruments and methods, preparation of sugar derivatives, steroids, etc., can solve problems such as deep color of products, reduce the content of impurities, reduce production costs, and improve purity. Effect

Active Publication Date: 2011-12-14
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The tea saponin product purity that this method gained is higher, re

Method used

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  • Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling
  • Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling
  • Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] HPLC Analysis Method of Tea Saponin in Camellia oleifera

[0050] Method 1: Using UV detection method

[0051] (1) Chromatographic conditions: column C 18 ODS (Φ4.6mm×200mm, 5μm), mobile phase: methanol-water (containing 0.05% glacial acetic acid) volume ratio 6:4, detection wavelength 210nm, flow rate 1ml / min.

[0052] (2) Standard curve drawing: get 0.1g of tea saponin standard substance, dissolve in 100ml volumetric flask with 80% ethanol, make tea saponin standard substance solution concentration be 1mg / ml. Take standard solutions 1, 2, 3, 4, and 5ml respectively in 10ml volumetric flasks to prepare standard solutions of 0.1, 0.2, 0.3, 0.4, and 0.5mg / ml. Using 80% ethanol solution as a blank, draw a standard curve, the standard curve equation is y=1.6658x-0.7123, r=0.9995.

[0053] (3) Determination of sample purity: Get tea saponin crude product and refined product 0.5g respectively, dissolve in 50ml volumetric flask with 80% ethanol, measure according to the ab...

Embodiment 2

[0059] vacuum extraction

[0060] Using degreased camellia oleifera cake as raw material, extracting tea saponin by boiling under reduced pressure, using 60-90% ethanol as extraction solvent, the ratio of extraction solvent to camellia oleifera cake is 1-30:1, preferably 5-15: 1. The extraction time is 4-30min, preferably 8-15min, the extraction temperature is 20-70°C, preferably 40-60°C, the extraction pressure is 0.01-0.08MPa, preferably 0.03-0.06MPa, and the extraction is 1-4 times, preferably 2 ~3 times, the extraction rate of camellia saponin is greater than 90%.

[0061] The present invention has studied the influence of extraction pressure, alcohol concentration, solid-liquid ratio and extraction time on tea saponin extraction rate, has designed 4 factors 4 levels [L 16 (4 4 )] Orthogonal test, with the extraction rate of tea saponin as an index to investigate the decompression boiling extraction process, the test results are shown in Table 1 and Table 2.

[0062] Ta...

Embodiment 3

[0068] Membrane purification process

[0069] The extract is formulated into a feed solution with a concentration of 1% to 4%, and the above feed solution is filtered with a ceramic membrane with a pore size of 0.05 μm to 0.2 μm, preferably with a membrane pore size of 0.05 μm, and an operating pressure of 0.15 to 0.3 MPa, preferably 0.15 to 0.3 MPa. 0.15MPa, the tea saponin solution passed through the ceramic membrane is decompressed and the ethanol is recovered to a solution containing 1-3g / ml of raw materials.

[0070] The present invention selects 0.2 μm, 0.1 μm, and 0.05 μm membrane aperture to investigate the influence of membrane aperture on membrane flux, tea saponin transfer rate and impurity removal rate, the results are as follows image 3 , Figure 4 shown. It can be seen from the figure that the membrane flux decreases to varying degrees with the extension of membrane filtration time. The results show that the membrane flux, tea saponin transfer rate and impuri...

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Abstract

The invention relates to a method for extracting high-purity tea saponin from an oil-tea-cake by decompression boiling. In the method, a degreased oil-tea-cake is used as a raw material, hydrous ethanol is used as an extraction solvent, and decompression boiling is adopted for extraction; after being filtered, extract passes through a ceramic membrane; ethanol is recovered from the tea saponin solution passing through the ceramic membrane, and the tea saponin solution is concentrated; and the concentrated solution is adsorbed through macroporous resin and chromatographically separated by medium and low pressure columns to prepare the high-purity tea saponin. The tea saponin prepared by adopting the technology has light color and high purity of over 95 percent, and the method becomes a novel technology for producing tea saponin product in the industry.

Description

technical field [0001] The invention relates to the technical field of plant extracts, in particular to a method for extracting high-purity tea saponin from camellia oleifera cake by boiling under reduced pressure. Background technique [0002] Camellia oleifera (Camellia Oleiferal Abel.) is a plant of the genus Camellia in the family Theaceae. Camellia oleifera in my country is rich in resources, mainly distributed in Hunan, Hubei, Jiangxi, Anhui and other provinces in China. Camellia oleifera seeds are called camellia cakes, and tea saponin mainly exists in camellia cakes. There are at least 1 million tons of camellia cake resources in my country every year, and at least 200,000 tons of tea can be produced every year by using them. Saponin. If we can fully extract and separate high-purity tea saponin, and comprehensively utilize the camellia oleifera cake, we can turn waste into wealth, increase farmers' income, and benefit environmental protection, producing considerable...

Claims

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Application Information

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IPC IPC(8): C07J63/00C07H15/256C07H1/08
Inventor 王成章周昊
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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