Method for extracting active ingredients from tangerine seeds

A technology for active ingredients and orange pits, applied in the field of extraction and separation of active ingredients of natural products, can solve the problems that the extraction and purification process needs to be perfected, the extraction method goes against objective facts, the yield of limonin is low, and the like, so as to avoid flammability. Explosive problem, short extraction time, high yield effect

Inactive Publication Date: 2011-08-17
BEIHANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are three main problems in the technology of extracting active ingredients from orange stones: first, the extracted limonin has a low yield or low purity, and the extraction and purification process needs to be perfected; secondly, a large amount of Organic solvents such as sherwood oil, acetone, ethyl acetate and ethanol are used as degreasing or extraction solvents, and these organic solvents pollute the environment, and are inflammable and explosive, and are difficult to preserve; again, the current method only extracts the single component of orange stone Separation, failing to organically combine the extraction and separation of various active ingredients in the orange core, thus increasing the production cost
For example, the patent with the publication number CN101367823A: The method for separating limonin, evodiamine and evodiamine from Evodia rutaecarpa: It is recorded that limonin with a purity of

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  • Method for extracting active ingredients from tangerine seeds
  • Method for extracting active ingredients from tangerine seeds
  • Method for extracting active ingredients from tangerine seeds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] A method for extracting active ingredients from tangerine stones, specifically comprising the following steps:

[0072] The first step: extract the orange oil after crushing the orange core:

[0073] After 42.74g orange core is pulverized to 60 orders, join in supercritical carbon dioxide extractor and extract orange oil, set carbon dioxide gas pressure as 30MPa, extraction temperature is 48 ℃, extraction time is 1.5 hours, obtains orange oil 17.74g and de-orange orange Nuclear residue 24.98g.

[0074] The second step: remove the oil orange pit residue and soak and homogenate:

[0075] According to the ratio of liquid to solid ratio of 10ml / g, use distilled water to soak to remove oil orange core residues, and adjust the pH value to 8 with a NaOH solution with a concentration of 3M. After soaking for 0.5h at a temperature of 80°C, use a flash extractor. For homogenization treatment, the rotation speed is 3500r / min, stirring and crushing for 3min, and a homogenate liqu...

Embodiment 2

[0092] The difference between this example and Example 1 is that it includes the process of preparing limonin acidic aglycone, specifically:

[0093] Dry the supernatant C obtained by centrifuging in the eighth step under reduced pressure. The drying conditions under reduced pressure are 0.08MPa and 80°C to obtain the crude limonin acid aglycone, which is then extracted with methanol and evaporated at 40°C. Methanol was recovered to obtain 0.21 g of limonin acid aglycone as the extract.

Embodiment 3

[0095] The difference between this embodiment and Example 2 is that it also includes the steps of preparing nomilin and limonin neutral aglycone, specifically:

[0096] Evaporate the mother liquor A in the ninth step to dryness to obtain a dry product, add methanol (analytical pure) to the dry product according to the ratio of liquid to solid ratio of 15ml / g, then stand at -20°C for 0.5h, and centrifuge at 4000r / min for 10min , the precipitate obtained is crystal B, the supernatant is mother liquor B, and the crystal B is 0.036 g of nomilin. .

[0097] After the mother liquor B was evaporated to dryness, the crude limonoid neutral aglycone was obtained, and NaOH with a pH value of 10 was added to the crude limonoid neutral aglycone at a liquid-solid ratio of 8ml / g, and heated to 60 ℃ to dissolve the crude limonin neutral aglycone in NaOH solution with a pH value of 10, and then use 4M hydrochloric acid to adjust the pH of the solution to 1.5, centrifuge, and wash the obtained...

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Abstract

The invention provides a method for extracting active ingredients from tangerine seeds. The method comprises the following steps of: crushing the tangerine seeds, performing supercritical extraction of tangerine oil, performing immersion and homogenizing treatment on oil-removed tangerine seed residue, performing centrifugal separation on the homogenate, performing ultra-filtration treatment on supernate A, and performing affinity chromatography on filtrate and the like to finally obtain limonin with high purity and other active ingredients such as acidic limonin aglycon, nomilin, neutral limonin aglycon (containing no limonin or nomilin) and the like extracted from the waste tangerine seeds so as to realize comprehensive utilization of a tangerine seed resource. The method has high yield, the consumption of an organic solvent is greatly reduced in the extraction process, the flammable and combustible problems caused by extraction with the organic solvent are avoided, the production cost is reduced, and the environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of natural product active ingredients, and in particular relates to a method for extracting active ingredients from orange pits. Background technique [0002] Limonin analogues are a class of biologically active ingredients in orange pits, mainly including limonin acid aglycone, limonin, nomilin, limonin neutral aglycone (excluding limonin and nomilin) , all belong to triterpenoids, and have significant effects in promoting cancer cell apoptosis, regulating low-density lipoprotein, treating colon cancer, antibacterial and insecticidal, etc. Therefore, the application and development of limonin analogues has great medical value and Broad market prospects. [0003] At present, the extraction and separation process of limonin and its analogues requires a large amount of organic solvents and low yield. In addition to cost factors, my country is still unable to realize the large-scal...

Claims

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Application Information

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IPC IPC(8): C07J73/00C11B1/10
CPCY02P20/54
Inventor 荣龙刘灿刘静荣永海黄国伦
Owner BEIHANG UNIV
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