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Separation and purification method of limonin compound C in Fructus Swietenia Macrophylla

A technology for the separation and purification of limonoids, which is applied in the direction of organic chemistry, can solve the problems of low extraction rate and cumbersome extraction methods, and achieve the effects of high extraction rate and purity, short time and simple operation

Inactive Publication Date: 2019-11-08
长沙市望城区产商品检测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the currently reported method for extracting and separating limonoid compound C from Xiangtianguo uses multiple extractions, multiple column chromatography and preparative liquid phases. This extraction method is cumbersome and the extraction rate is low.

Method used

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  • Separation and purification method of limonin compound C in Fructus Swietenia Macrophylla
  • Separation and purification method of limonin compound C in Fructus Swietenia Macrophylla
  • Separation and purification method of limonin compound C in Fructus Swietenia Macrophylla

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 50g of dried Xiangtianguo, crush it through a 200-mesh sieve to obtain powder; add the powder to 250mL methanol, extract for 2 hours with a Soxhlet extractor, filter, and take the supernatant; add the supernatant to 500g macropore In the adsorption resin XDA-7, adsorb for 3 hours, wash the resin column three times with 1.5L of water, and then elute with a mixed solvent of ethanol-acetone-n-hexane with a volume ratio of 6:3:1, collect the eluate, and concentrate under reduced pressure. Obtain the initial product; the initial product is dissolved with 20mL of ethanol under reflux, placed to crystallize, filtered and then washed twice with petroleum ether and dried to obtain 0.12g of white powder limonoid compound C, and the reference standard is detected by high performance liquid phase. The characteristic front positions are the same, and the calculated content is 95.2%. MS: 503.2[M+H] + . 1 H-NMR (CDCl 3 ,300MHz) δ: 2.10d(3-OH), 2.58br s(1-OH), 2.96br s(6-OH). ...

Embodiment 2

[0024] Take 100g of dried Xiangtianguo, crush it through a 200-mesh sieve to obtain a powder; add the powder to 500mL of ethanol, use a Soxhlet extractor to extract for 3 hours, filter, and take the supernatant; add the supernatant to 1kg macropore In the adsorption resin XDA-7, adsorb for 2 hours, wash the resin column three times with 3L of water, and then elute with a mixed solvent of ethanol-acetone-n-hexane with a volume ratio of 6:3:1, collect the eluate, and concentrate under reduced pressure to obtain The initial product: the initial product was dissolved with 40 mL of ethanol under reflux, placed to crystallize, filtered, washed twice with ether and dried to obtain 0.25 g of white powder limonoid compound C, the content of which was 94.5% by HPLC.

[0025] Screening experiment of elution solvent: the same method as in Example 2 was adopted, the difference being that the type and ratio of the elution solvent were replaced, and the results obtained are shown in Tables 2 ...

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Abstract

The invention belongs to the extraction field of limonin compounds, and particularly relates to a method for extracting limonin compound C from Fructus Swietenia Macrophylla. In the method, dried Fructus Swietenia Macrophylla is taken as a raw material, crushed, extracted by an alcohol solvent, adsorbed by macroporous resin, eluted by a mixed solvent, crystallized, washed and dried to obtain the limonin compound C with higher purity. The method has the advantages of simple operation, short time, high extraction rate, high product purity and the like.

Description

technical field [0001] The invention belongs to the field of extraction of limonoid compounds, in particular to a method for separating and purifying limonoid compound C from Xiangguo. Background technique [0002] Xiangtian fruit is the fruit of the large-leaved mahogany plant in the Meliaceae family. It is rich in the Solomon Islands in the South Pacific and is widely used as a traditional folk medicine in the area where it is rich. The bark, leaves, fruit and seed oil of the celestial fruit plant have good functional activities, and the celestial fruit is mainly used as a folk medicine for the treatment of diseases such as hypertension, hyperglycemia, malaria, intestinal parasitic infection and cancer and conditioning. Research reports have shown that both the monomeric components and extracts of Xiangtianguo have obvious pharmacological effects, and the main components in the fruit are limonin. Limonoids are a class of triterpenoids with good activity. They are widely ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 徐步城熊鼎程丹
Owner 长沙市望城区产商品检测中心
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