Extraction and separation technology and production process of limonin glucoside

A limonin glycoside and separation technology, which is applied in the field of limonin glycoside extraction and separation technology and production technology, can solve the problems of high performance liquid chromatography, such as limited preparation, high price, and product yield decline, and achieve a large The effect of competitive advantage

Active Publication Date: 2014-03-26
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are some defects in the above separation methods. First, resin XAD-2 is used in these separation methods. The price of this kind of resin is extremely expensive, and industrial production cannot be realized at all; secondly, 4-5 times of column chromatography are usually required in these methods It can only be completed, the operation is more cumbersome, and it will bring huge energy and raw material loss during industrialization; thirdly, due to the large number of operations, it has brought the disadvantage of a sharp drop in product yield; finally, the final purification stage of these methods uses preparation. High-performance liquid phase purification method, otherwise the product purity cannot meet commercial needs, and the preparation amount of high-performance liquid chromatography is extremely limited, so technical innovation is required

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) Crush and sieve: take 60 kg of orange core and crush it and pass it through a 10-16 mesh sieve.

[0015] (2) Extraction: Soak in 5 times the amount of 10% ethanol for two hours, extract for 1.5 hours, and extract twice.

[0016] (3) Concentration under reduced pressure: filter after extraction, concentrate under reduced pressure and filter the liquid, then centrifuge at 2000 rpm for 30 minutes, and extract about 35 liters of the middle layer of the clarified liquid. Add 4 times the amount of methanol, heat under stirring conditions for 30 minutes, condense and ethanol precipitation for 24 hours, extract the supernatant liquid, filter the precipitate under reduced pressure, combine the supernatant and filtrate, and dry the combined liquid under reduced pressure to obtain a dry cream About 2 kg.

[0017] (4) Resin adsorption: The present invention has investigated 10 kinds of resins including XAD series, LX series, HB series, ZSA series, etc., and found that ZSA-550 ...

Embodiment 2

[0023] (1) Crushing and sieving: take 120 kilograms of orange cores, pass through a 10-16 mesh sieve after crushing.

[0024] (2) Extraction: soak in 500 kg of 20% ethanol for two hours, and extract continuously for 1.5 hours.

[0025] (3) Concentration under reduced pressure: Concentrate the filtered solution under reduced pressure to 80 kg, then centrifuge at 2000 rpm for 30 minutes, and extract about 60 liters of the middle clarified liquid. Add 4 times the amount of methanol, heat under stirring conditions for 30 minutes, condense and ethanol precipitation for 24 hours, extract the supernatant liquid, filter the precipitate under reduced pressure, combine the supernatant and filtrate, and dry the combined liquid under reduced pressure to obtain a dry cream About 4 kg.

[0026] (4) Resin adsorption: The present invention has investigated 10 kinds of resins including XAD series, LX series, HB series, ZSA series, etc., and found that ZSA-550 resin has the best effect, which ...

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PUM

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Abstract

The invention relates to an extraction and separation technology and a production process of limonin glucoside. A limonin substance is a triterpene ingredient existing in rutaceae and meliaceae plants, has anti-inflammatory and analgesic effects and an effect of resisting various cancer cells and is mainly applied to food additives and cosmetics. But the flavor of the limonin substance is bitter, and the solubility is poorer, so that the wide application of the limonin substance is limited. The limonin glucoside is an advanced glycation end product of limonin, has the characteristics of no foreign flavor, good solubility, solution stability and the like and has a wider market prospect. An extraction process of the limonin glucoside is as follows: crushing and sieving, reflux extraction and concentration, alcohol precipitation, impurity removal, resin separation, decolorization, column chromatography and detection. The natural content of the limonin glucoside is about 0.02%. By the aid of the extraction and separation technology and the production process of limonin glucoside and a method, a target product can be effectively enriched, products with different specifications of 60%, 90%, 98% and the like are finally obtained, and the method is simple, convenient, feasible and suitable for industrialization.

Description

technical field [0001] The invention relates to the field of limonoid glycosides, in particular to an extraction and separation technology and production process of limonoid glycosides. Background technique [0002] Limonoids are highly oxidized triterpenoids, mainly found in Rutaceae and Meliaceae plants, mainly represented by limonoids and nomilins. These two types of components were first reported in 1989. Lam and Hasegawa had reported that nomilin components had the effect of inhibiting benzo (α) pyrene-induced gastric gastric tumors in mice; Miller had reported that limonoids and nomilin Mirin-like components all have the effect of reducing 7,12-dimethylbenzo(α)anthracene-induced epidermoid carcinoma in the cheek pouch of female Syrian hamsters, and these two types of components have anticancer, antiviral, anxiolytic and insecticidal effects. etc. have strong biological activity, but they have not been widely commercialized because of their extremely bitter taste and p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/26C07H1/08
Inventor 张起辉孙宗良石徐程孟霞杜浩张忠山
Owner CHONGQING UNIV
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