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Process for extracting limonin from shaddock kernel

A technology of limonin and pomelo core, which is applied in the field of biochemical separation and purification, can solve the problems of high cost, complicated process and low content, and achieves the effects of low cost and simple process

Active Publication Date: 2009-09-16
HUACHANG POLYMER EAST CHINA UNIV OFSCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology can separate limonoid analogs, but the content is not high, and can not separate limonoid monomer
[0005] To sum up, the existing technology is complicated in process and high in cost, and it is mostly used in laboratories and cannot be mass-produced.

Method used

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  • Process for extracting limonin from shaddock kernel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The pomelo cores washed with water were placed in a drying oven at 65°C for 7 hours until the weight was reached, and then crushed to 20 mesh to obtain powder. Weigh 60 grams of pomelo seed powder, wrap it with filter paper, place it in a Soxhlet extractor, and extract 30 times continuously with 300 ml of 60% ethanol aqueous solution at a temperature of 100°C. The extract was diluted to ethanol concentration of 50%, the pH of the extract was 3.0, and flowed through a 50ml HZ816 resin column at a flow rate of 1ml / min. First rinse with 200ml of 40% ethanol aqueous solution at a flow rate of 1ml / min, discard the eluent, then elute with 300ml of 70% ethanol aqueous solution at a flow rate of 1ml / min, collect the eluate, and distill under reduced pressure (0.8bar , 80°C), concentrated to dryness, dissolved in 20ml of dichloromethane, filtered, added 40ml of isopropanol, placed in a refrigerator at 4°C, and slowly stirred for crystallization. The crystallization solution was...

Embodiment 2

[0028] The macroporous adsorption resin HZ816 in Example 1 was replaced with HZ818, and the others were the same as in Example 1 to obtain about 150 mg of limonin finished product with a purity of 92.5%.

Embodiment 3

[0030] Put the washed pomelo cores in a drying oven at 60° C. for 8 hours until the weight is reached, and crush the dried pomelo cores to 40 meshes to obtain powder. Weigh 60 grams, wrap it with filter paper, put it in a Soxhlet extractor, and extract 25 times continuously at a temperature of 110° C. with 300 ml of 70% ethanol aqueous solution. The extract was diluted to an ethanol concentration of 50%, the pH of the extract was 4.0, and flowed through a 50 ml HZ818 resin column at a flow rate of 1 ml / min. Wash with 150ml of 45% ethanol aqueous solution respectively, and the flow rate is 1ml / min. The eluate obtained is discarded, and then eluted with 250ml of 80% ethanol aqueous solution, and the flow rate is 1ml / min. The eluent is collected, and the vacuum distillation (0.8bar , 80°C), concentrated to dryness, dissolved in 20ml of dichloromethane, filtered, added 40ml of isopropanol, placed in a refrigerator at 4°C, and slowly stirred for crystallization. The crystallizatio...

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Abstract

The invention provides a process for extracting limonin from a shaddock kernel. The process is characterized in that the process comprises the following steps that: (1) pre-treatment of shaddock kernel: after washing and drying, the shaddock kernel is crushed to be between 20 and 40 meshes; (2) extraction: by taking a water solution of ethanol as a solvent, the shaddock kernel powder is subjected to thermal refluxing extraction at a temperature of between 90 and 100 DEG C; (3) impurity separation: the obtained product after thermal refluxing extraction is orderly impurity-separated by macroporous occluded resin, leached by 30 to 50 percent water solution of ethanol and eluted by 60 to 80 percent water solution of ethanol, and the leaching liquid is abandoned, and the eluate is collected; and (4) the collected eluate is condensed until being dry and dissolved by methylene chloride and filtered; the obtained product is added with isopropyl alcohol which is doubled in volume than the obtained product, cooled down to the temperature of 4 DEG C, and slowly stirred for crystallization; and the crystal is filtered and dried to obtain the finished product. The process has the advantages that by utilizing the processes of thermal refluxing extraction, impurity separation by occluded resin, and the like, the limonin with the content of over 90 percent can be extracted from the shaddock kernel; moreover, the process also has the advantages of simple process, recoverable leaching agent, low cost and mass production.

Description

technical field [0001] The invention belongs to the technical field of biochemical separation and purification, and in particular relates to a process for separating, purifying and extracting limonin from pomelo seeds. Background technique [0002] Limonin (limonin) is Phellodendron lactone, also known as rutaecarin and albinolactone, is a secondary metabolite of triterpenoids, mainly found in Rutaceae and Meliaceae plants. The grapefruit fruit belonging to Rutaceae contains limonin, and the pomelo core has the largest content. Limonin has anti-cancer, analgesic, deworming and insecticidal effects, regulates cholesterol levels in the body, and prevents atherosclerosis. Therefore, the separation and purification of limonin has attracted the attention of biochemical researchers, and there have been reports on the technology of separation and purification of limonin in the literature. [0003] Chinese patent CN1279242A provides a process for extracting limonin from Rutaceae f...

Claims

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Application Information

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IPC IPC(8): C07D493/22A61K36/752
Inventor 江邦和王辉徐环昕宁方红张磊刘坐镇
Owner HUACHANG POLYMER EAST CHINA UNIV OFSCI & TECH
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