Extraction and preparation method for limonin components

A technology of limonin and extract, which is applied in the field of biomedicine and can solve problems that have not yet been discovered

Inactive Publication Date: 2015-08-19
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Extraction and preparation method for limonin components

Examples

Experimental program
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Effect test

experiment example 1

[0029] Experimental example 1: Determination of total citrin content.

[0030] 1. Preparation of reagents

[0031] (1) Limonin standard solution: Accurately weigh 0.0092g of limonin with an electronic balance, dissolve it with an appropriate amount of distilled water, transfer it to a 50mL volumetric flask after dissolving, constant volume, and shake well to obtain a mass concentration of 184mg / L Limonin standard solution;

[0032] (2) Display agent: Measure 65mL of concentrated sulfuric acid and 35mL of absolute ethanol, mix them, and add 125mg of p-dimethylaminobenzaldehyde after cooling. When in use, add 0.05mL of 9% ferric chloride solution to the solution and mix it evenly, and prepare it now;

[0033] (3) 9% ferric chloride solution: Weigh 4.5 g of ferric chloride solid, dissolve the solid in 45.5 mL of distilled water, and transfer it to a brown reagent bottle for storage after cooling.

[0034] 2. Make a standard curve

[0035] Take 6 test tubes, add 0, 0.4, 0.8,...

experiment example 2

[0038] Experimental example 2: HPLC-MS qualitative analysis of the total limonin extract of Ragbu japonica.

[0039] Preparation of the sample solution: take the total limonin extract of the ragwort fruit, prepare the test solution with methanol, filter it with a 0.45um organic microporous membrane, and use it as the test solution.

[0040]Preparation of standard solution: take homemade limonin, nomilin, limonoid diomol, leucodiol, 1-deacetylniporin B, cortex ketone, Yichangsu, granatumin H, swimacronoid A , add an appropriate amount of methanol as a standard solution.

[0041] Instrument: German Thermo Fischer Scientific high-resolution liquid chromatography-mass spectrometer.

[0042] Chromatographic conditions: Waters Symmetry C18 column (5μm, 250mm × 4.6mm), column temperature: 25°C, flow rate 800μl / min, detection wavelength: 550nm, injection volume: 5ul. Mobile phase: use acetonitrile as mobility A, 0.1% ammonia water as mobility B, carry out gradient elution as specifi...

Embodiment 1

[0047] Example 1: Preparation of total limonin extract and monomeric compound of Ragbukia

[0048] (1) 15kg of Ragwood fruit, use 80% ethanol as solvent, extraction temperature is minus 7°C, extraction times are 3 times, each extraction time is 7 hours, each time the amount of solvent is 15 times of the weight of Ragwood fruit, Filtrate, and freeze-dry the extract to obtain the crude extract of Ragbukia fruit;

[0049] (2) Purify the crude extract of Ragbukia fruit obtained in step (1) through MCI gel column chromatography, first elute with methanol-water with a part ratio of 2:98, and then use a part ratio of 10:90 Methanol-water elution, collect the methanol-water elution part with a fraction ratio of 10:90, recover methanol, and dry to obtain the ragwort fruit extract;

[0050] (3) Put the ragwort fruit extract obtained in step (2) through an MCI gel-silica gel mixed chromatographic column with a weight ratio of 1:1, and use petroleum ether-acetone gradient elution, and us...

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Abstract

The invention discloses a method for preparing a total limonin extract of a cordia dichotoma fruit. The total limonin extract of the cordia dichotoma fruit is prepared according to the following method comprising the steps: extracting the cordia dichotoma fruit, serving as a raw material, at low temperature by using 75 to 100 percent of ethyl alcohol, and purifying the cordia dichotoma fruit through MCI gel column chromatography and the like to obtain the total limonin extract of the cordia dichotoma fruit.

Description

technical field [0001] The invention belongs to the field of biomedicine, and relates to a method for extracting and preparing limonoid components, in particular to a method for preparing total limonin extract from ragwort. Background technique [0002] Cordia dichotoma Forst.f. Picked when the fruit is ripe in autumn, and dried in the sun. flat nature. Included in 1998 "Ministry of Health of the People's Republic of China Drug Standards Uighur Drug Sub-volume". It has the functions of maturing and clearing abnormal mucus, regulating the balance of bile, moisturizing the lungs and relieving cough, widening the chest and resolving phlegm. It is used for persistent cough, strong biliary fluid, unpleasant expectoration, dry throat and itchy throat. Textual research "Garden of Medicine" contains: "The ragwood fruit is the fruit of a tree with a height of 2-10m, off-white bark, light yellow branches, round leaves, larger, leathery; the shape of the fruit is similar to the nip...

Claims

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Application Information

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IPC IPC(8): A61K36/30A61K131/00
Inventor 韩俊芬赵莹曹明亮
Owner TAISHAN MEDICAL UNIV
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