Extraction method for comprehensive utilization of schisandrae chinensis

An extraction method, the technology of Schisandra chinensis, applied in the field of comprehensive utilization of Schisandra chinensis extraction, can solve the problems of unsatisfactory antibacterial effect and waste of supercritical extracts

Inactive Publication Date: 2017-09-01

HUNAN NUOZ BIOLOGICAL TECH CO LTD

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AI-Extracted Technical Summary

Problems solved by technology

Unsaturated fatty acids with economic value such as linoleic acid and oleic acid in Schisandra chinensis are finally discarded together with the extraction residue, resulting in waste

It was found that the inhibitory effect of alcohol extract and water extract on Esc...

Method used

(2) effectively separate polysaccharide and organic acid in Fructus Schizandra by nanofiltration membrane, easy and simple to handle, and reduced the impurity in Fructus Schizandra polysaccharide part, avoided the use and loss of ethanol, reduced energy consumption; In addition, with Compared with boiling at high temperature, the way of extracting Schisandra fruit with warm water avoids or reduces the loss of heat-sensitive lignans;

(3) subcritical extraction and molecular distillation technology are used in combination, which has the advantages of simple operation technology, beneficial to industrialized large-scale production, low cost, energy saving and environmental protection;

[0029] The extraction of Schisandra water-soluble polysaccharide components generally adopts the method of water extraction and alcohol precipitation. But this way has some disadvantages. For example, the method of alcohol precipitation to separate polysaccharides has the problem of incomplete precipitation of small molecule polysaccharides; it also leads to impurities such as inorganic salts and proteins in the polysaccharide precipitation, which usually need to be removed after repeated alcohol precipitation processes. The large amount of ethanol used, the energy consumption in the ethanol recovery process, and the waste of ethanol caused by incomplete recovery lead to high costs. The method of the present invention is based on the molecular weight difference between the macromolecular Schisandra polysaccharide and the small molecular water-soluble organic acid, and realizes the separation of the two by using a nanofiltration membrane with an appropriate pore size, so the operation is simple, and the impurities in the Schisandra polysaccharide part are reduced. The u...

Abstract

The invention relates to an extraction method for comprehensive utilization of schisandrae chinensis. The method is characterized by including the steps of: (1) extraction of schisandra chinensis polysaccharide and water-soluble organic acid from fructus schisandrae chinensis; and (2) extraction of schisandrae chinensis lignans and schisandrae chinensis oil from schisandrae chinensis residue obtained by step (1).

Application Domain

Plant ingredients

Technology Topic

Organic acidChemistry +5

Image

Examples

Experimental program(3)

Example Embodiment

[0063] Example 1:

[0064] Take 100Kg of dried fruit of Schisandra chinensis, add 10 times (v/w) and 8 times (v/w) of water to soak twice at 60°C for 2 hours each time. Combine the soaking liquid and pass through 0.25um pore size inorganic ceramics. Membrane filtration, and the filtrate is filtered with a nanofiltration membrane with a molecular weight cut-off of 2000 Daltons. The filtrate is concentrated under reduced pressure, mixed with 2Kg of medicinal starch, and spray-dried to obtain 19Kg of brown dry powder containing Schisandra organic acid. The content of organic acid is 43.15%.

[0065] Add 2 times the volume of water to the remaining liquid, filter with a nanofiltration membrane with a molecular weight cut-off of 2000 Daltons, discard the filtrate, and spray dry the remaining liquid to obtain 5.9Kg of Schisandra polysaccharide fraction, which is a light brown powder, of which Schisandra The total polysaccharide content is 57.91%.

[0066] Dry the soaked schisandra (i.e. schisandra residue), pulverize it into coarse powder, add 8 times (v/w) and 6 times (v/w) of 80% ethanol for reflux extraction twice, each for 2 hours , Combine the extracts, filter with an inorganic ceramic membrane with a pore size of 0.25um, concentrate the filtrate under reduced pressure, add 12Kg of water-soluble starch to the resulting extract, mix it, and dry it under vacuum to obtain 21.1Kg of product containing Schisandra lignans. It is light brown yellow powder. The content of total lignans in the product measured by high performance liquid chromatography (HPLC) was 15.96%.

[0067] The extraction residue from the recovered ethanol is dried in the sun, and then propane is used as the extractant, and the subcritical extraction is carried out at 50°C and 3.0-5.0MPa pressure at a ratio of 1:3.3 (w/v) to a total of 3 extractions. , The extraction time is 45 minutes each time, and the extracts are combined to obtain 24.7Kg of crude schisandra oil. Then the crude schisandra oil was molecularly distilled under a vacuum of 2~3 Pa and a temperature of 200~210℃, and 21.4Kg of schisandra oil was obtained, which was a clear yellow-brown liquid. The content of linoleic acid was measured by gas chromatography. 75.58%.

Example Embodiment

[0068] Example 2:

[0069] Put about 13.0Kg of schisandra oil obtained in Example 1 and distilled water into a flat-bottomed flask at an oil:water ratio of 2:1.3 to 2:1.5, slowly increase the temperature to 80-85°C with stirring, and slowly drop 40% NaOH Solution, make the final pH value of the reaction solution reach 12, stir and keep the reaction temperature for 5-6 hours, then transfer it to a separatory funnel, stand still for layering, and remove the lower layer of glycerin. Transfer the treated reaction solution to a flat-bottomed flask again, slowly raise the temperature to 90-95°C, slowly drop in 28% sulfuric acid solution to make the final pH of the reaction solution 2, and keep the reaction for 4 to 5 hours, then transfer to a separatory funnel. Wash with distilled water at 60-70°C until it is neutral. After standing for stratification, remove the lower water layer to obtain 12.1Kg of crude fatty acid.

[0070] 6.1Kg of urea was added to a certain amount of anhydrous methanol, heated to reflux, so that all the urea was dissolved to form a saturated solution (methanol:urea=about 2:1). First take 1/2 of the saturated solution, add the obtained crude fatty acid to react (generally stir and reflux on a water bath for about 40 minutes), then place it at room temperature for about 12 hours, and filter with suction. Then, add 1/2 of the remaining urea saturated solution to the filtrate for reaction, place it at 0-4°C for 8-10 hours, and filter with suction. Finally, all the remaining saturated urea solution was added to the filtrate for reaction, placed at -10°C for 5-6 hours, and filtered with suction. The filtrate was vacuum rotary evaporated at 30°C to remove methanol, and then washed with distilled water at 40-50°C. After standing still, the water layer was removed to remove urea, and 10.1Kg of product was obtained, which was a clear yellow-brown liquid, in which linoleic acid The content is 95.09%.

Example Embodiment

[0071] Example 3:

[0072] Take 100Kg of dried fruit of Schisandra chinensis, add 10 times (v/w) and 8 times (v/w) of water to soak twice at 60°C for 2 hours each time. Combine the soaking liquid and pass through 0.25um pore size inorganic ceramics. Membrane filtration, the filtrate is filtered with a nanofiltration membrane with a molecular weight cut-off of 2000 Daltons, the filtrate is concentrated under reduced pressure, 2Kg of medicinal starch is added, and spray-dried to obtain a brown dry powder containing Schisandra organic acid 19.1Kg, of which The total organic acid content is 44.76%.

[0073] Add 2 times the volume of water to the remaining liquid, filter with a nanofiltration membrane with a molecular weight cut-off of 2000 Daltons, discard the filtrate, and spray dry the remaining liquid to obtain 5.3Kg of Schisandra polysaccharide, which is a light brown powder. The content of polysaccharide is 52.23%.

[0074] The soaked schisandra (i.e. schisandra residue) is dried, crushed into coarse powder, and then propane is used as the extractant, and the subcritical extraction is carried out at 50°C and 3.5-5.0 MPa at a material-to-liquid ratio of 1:3.3. The extraction was performed 4 times, and the extraction time was 45 minutes each time to obtain 35.8Kg of oily extract. Then, the oily extract is molecularly distilled under a vacuum of 2 to 3 Pa and a temperature of 200 to 210°C to obtain 21.4Kg of a heavy oily extract, which is the oil part of schisandra and is a clear yellow-brown liquid; The oily extract 13.6Kg, which is the lignan part of Schisandra, add 16Kg of water-soluble starch to it, mix and dry in vacuum, then 29.5Kg product containing the lignan part of Schisandra is obtained, which is yellow to light yellow powder. The content of total lignans in the obtained product measured by high performance liquid chromatography (HPLC) was 13.12%.

[0075] The schisandra oil part contains saturated fatty acids palmitic acid and stearic acid, and unsaturated fatty acids linoleic acid, oleic acid and linolenic acid. Gas chromatography was performed on the schisandra oil part, and data processing was performed. Gas chromatogram such as figure 1 As shown, the analysis results are shown in the following table.

[0076]

[0077] As shown in the table, the contents of linoleic acid, oleic acid, palmitic acid, linolenic acid, and stearic acid in the schisandra oil part are about 75.66%, 15.66%, 1.95%, 0.60% and 0.40%, respectively.

PUM

Property	Measurement	Unit
Molecular weight	1000.0 ~ 5000.0

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