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Method for extracting limonin and nomilin

A technology of limonin and nomilin, applied in steroids, fermentation, organic chemistry, etc., can solve the problems of large amount of organic solvent, low extraction yield, and high extraction cost

Active Publication Date: 2018-10-12
北京颐方生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the problems existing in the above-mentioned limonin and nomilin extraction process, the present invention provides a method for extracting limonin and nomilin, which can promote the stripping of limonin and nomilin in orange cores , which solves the problems of large amount of organic solvent, low extraction yield and high extraction cost in the existing process of limonin extraction

Method used

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  • Method for extracting limonin and nomilin
  • Method for extracting limonin and nomilin
  • Method for extracting limonin and nomilin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] 1) Orange core pretreatment: select dry orange core without mildew, crush it with a pulverizer, pass through a 80-100 mesh sieve, and set aside.

[0064] 2) Degreasing treatment: take the crushed tangerine core and carry out degreasing treatment. The degreasing conditions are: the degreasing solvent is petroleum ether with a boiling range of 60°C to 90°C, the liquid-to-solid ratio is 5L / kg, and the temperature is 60°C in a water bath. 6h, after degreasing, the orange core pretreatment material is obtained.

[0065] 3) Preparation of barley koji compound enzyme solution: take wine koji, pulverize it with a pulverizer, and pass it through a 100-mesh sieve. Add a phosphate buffer solution with a pH of 6.0 for leaching, and the leaching conditions are as follows: the ratio of liquid to material is 2.5 L / kg, the temperature is 6° C., and the time is 12 hours. Then filter the extract with 4 layers of gauze and filter paper successively, centrifuge the filtrate at 10,000 rpm ...

Embodiment 2

[0073] Steps 1)-3) are the same as in Example 1.

[0074] 4) Enzymolysis treatment: get orange core pretreatment material and add wheat koji compound enzyme liquid to carry out enzymolysis, and its condition is: add the phosphate buffer solution that pH is 6.0, the ratio of liquid to material is 8L / kg, wheat koji compound enzyme liquid adds The amount is 5% of the total volume, the pH value of the solution is 6.2, the enzymolysis temperature is 42° C., stirred and extracted for 8 hours, and the supernatant is removed by centrifugation to obtain the enzymolysis base material.

[0075] 5) Water co-solvent extraction: adding a solvent to the above-mentioned enzymolysis base material for extraction, the extraction conditions are: the extraction solvent is a sodium salicylate solution of 1.7mol / L, the liquid-to-solid ratio is 7L / kg, and the temperature is 53°C. The time is 8h. The extraction process adopts a three-stage four-tank countercurrent extraction method, and the extract i...

Embodiment 3

[0079] Step 1)-4) is identical with embodiment 1

[0080] 5) Water co-solvent extraction: adding a solvent to the above-mentioned enzymolysis base material for extraction, the extraction conditions are: the extraction solvent is a sodium salicylate solution of 1.5mol / L, the liquid-to-solid ratio is 6L / kg, and the temperature is 52°C. The time is 8h. The extraction process adopts a three-stage four-tank countercurrent extraction method, and the extract is separated after the extraction is completed.

[0081] 6) Macroporous resin adsorption analysis: adjust the pH of the above extract to 5.0 with 1mol / L hydrochloric acid, and centrifuge at 4000rpm for 10min to separate the precipitate. The supernatant was taken for resin adsorption, and the pretreated XAD-6 macroporous adsorption resin was packed into a column (10.8×200cm), the resin loading capacity was 50L, and the flow rate was 50ml / min for adsorption; after the adsorption was completed, first Washing with 25% ethanol for 3...

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Abstract

The invention relates to a method for extracting limonin and nomilin. The method comprises the following steps: degreasing a raw material, and then subjecting the degreased raw material to enzymatic hydrolysis with a wheat koji compound enzyme solution; removing supernatant liquid to obtain an enzymatic hydrolysis base material; adding a sodium salicylate solution for extraction, and separating aliquid extract; adjusting the pH value of the extract to 4.6-5.0, loading a supernatant onto macroporous resin, carrying out elution by using an ethanol solution with a concentration of 20-25% so as to remove impurities, then carrying out elution by using an ethanol solution with a concentration of 85-90%, collecting eluates, recovering the ethanol, and carrying out drying to obtain an extract A;dissolving the obtained extract A with a mixed solution of dichloromethane and isopropyl alcohol by heating, carrying out filtering to remove insoluble matters, and then successively carrying out cooling and crystallized so as to obtain limonin crystals; and subjecting mother liquid to pressure-reduced evaporation to dryness so as to obtain an extract B, dissolving the obtained extract B with a mixed solution of ethyl acetate and ethanol by heating, carrying out filtering to remove insoluble matters, and then successively carrying out cooling and crystallized so as to obtain nomilin crystals.The extraction method of the invention is low in cost and high in yield and product purity, and reduces environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of extraction, separation and purification of active ingredients in natural plants, and in particular relates to a method for extracting limonin and nomilin. Background technique [0002] Limonin and Nomilin are the main limonoid compounds in citrus, which are secondary metabolites of triterpenoids, mainly found in Rutaceae and Meliaceae, especially in citrus Higher content in the seeds of the genus. Limonoid compounds in citrus cores mainly include limonoid compounds aglycones and glycosides, among which aglycones mainly include limonin, nomilin, phellodendron, isofortonic acid, etc., and glycosides are generally The D ring opens to add a sugar group. Limonin, alias: Phellodendron lactone, Evodia lactone, molecular formula C 26 h 30 o 8 , molecular weight 470.53, pure product is white, bitter, crystalline; nomilin, molecular formula C 28 h 34 o 9 , molecular weight 514.57, white powder, bitter taste...

Claims

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Application Information

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IPC IPC(8): C12P33/20C07J73/00
CPCC07J73/003C12P33/20
Inventor 石清东王正元陈赫岩王姣
Owner 北京颐方生物科技有限公司
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