Method for extracting Natsucitrine I

A technology of extracting liquid and resin column, applied in the field of separation of natural products, can solve the problem of less research on torcianine I, and achieve the effects of reducing the amount of extraction, large processing capacity and lowering cost.

Inactive Publication Date: 2013-12-25
NANJING TONGZE AGRI SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are few domestic researches on toxia orange Ⅰ, and it is still in its infancy.

Method used

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  • Method for extracting Natsucitrine I

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Experimental program
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Effect test

Embodiment 1

[0016] Take the root of big tangerine, crush it and take 10kg, reflux and extract 50kg60% methanol solution for 3 times (the third extraction solution will be used for the next extraction), add 1kg diatomaceous earth activated carbon (5:1) to the extraction solution for decolorization, filter out solid impurities, Recover methanol under reduced pressure, adjust pH to 7.5 with ammonia water in the concentrate, add 2LXDA-5 resin column for adsorption, wash the resin column with deionized water until neutral, take 10L of 30% methanol solution (pH9) to elute the active ingredients, and concentrate the eluent under reduced pressure. 200 ml of the concentrated solution was obtained, and the concentrated solution was added with 150 ml of chloroform to extract three times, the chloroform layer was concentrated to 100 ml, refrigerated and crystallized, and the crystal was dried to obtain the citronine I product with a content of 91.3%.

[0017]

Embodiment 2

[0019] Take the root of big tangerine, crush it and take 10kg, reflux and extract 70kg60% methanol solution twice, add 2kg diatomaceous earth activated carbon (10:3) to the extract to decolorize, filter out solid impurities, recover methanol under reduced pressure, and adjust the pH of the concentrated liquid ammonia water to 8. 5. Add 2L SPD450 resin column for adsorption, wash the resin column with deionized water to neutrality, take 6L of 40% methanol solution (pH8) to elute the active ingredients, and concentrate the eluent under reduced pressure to obtain 250ml of concentrated solution, which is extracted by adding 200ml of chloroform to the concentrated solution 2 The second time, the chloroform layer was concentrated to 80ml, refrigerated and crystallized, and the crystals were dried to obtain the citronine I product, with a content of 87.8%.

[0020]

Embodiment 3

[0022] Take the root of tangerine, crush it and take 10kg, 70kg 60% methanol solution reflux and extract twice, add 2kg diatomite activated carbon (10:3) to the extract to decolorize, filter out solid impurities, recover methanol under reduced pressure, and adjust the pH of the concentrated liquid ammonia water to 8, Add 2L of SPD450 resin column for adsorption, wash the resin column with deionized water until neutral, take 8L of 50% methanol solution (pH8) to elute the active ingredient, concentrate the eluent under reduced pressure to obtain 200ml of concentrated solution, add 200ml of chloroform to the concentrated solution for extraction twice, Concentrate the chloroform layer to 120ml, refrigerate and crystallize, and dry the crystals to obtain the citronine I product with a content of 90.8%.

[0023]

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PUM

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Abstract

The invention relates to a method for extracting Natsucitrine I. The method comprises the following steps of: crushing roots of Citrus tangerine, adding 5-8 times of 60-80% methanol solution and performing reflux extraction for 2-3 times; discoloring the extracting solution by using 1-2 percent of diatomite and activated carbon, recovering methanol under reduced pressure, regulating pH value of the concentrated solution, adding a weakly acidic cation exchange resin or a macroporous resin for adsorption, washing the resin column to be neutral through deionized water, eluting active ingredients by using the alkaline methanol solution, concentrating the eluent under reduced pressure, performing chloroform extraction for 2-3 times, concentrating chloroform to a small size, carrying out refrigeration and crystallization, and drying the crystal to obtain the Natsucitrine I. According to the method, the Natsucitrine I is enriched and separated by adopting a resin column, and the method is easy to operate and can be put into industrial production easily.

Description

technical field [0001] The invention belongs to the field of separation of natural products, in particular to a method for extracting citronine I. Background technique [0002] Natsucitrine Ⅰ (Natsucitrine Ⅰ) exists in the root of the Rutaceae (Rutaceae) red orange Citrus tangerina Hort.ex Tanaka, is an acridine alkaloid alkaloid, molecular formula C 15 h 13 NO 5 , the structural formula is 287.27, and the structural formula is: [0003] [0004] There are few existing methods for extracting alkaloids. Generally, methanol, ethanol, etc. are used as solvents, extracted by dipping, percolation and ultrasonic methods, concentrated and then added with acid to remove impurities, then extracted with ether or chloroform, alkalized and precipitated. Aluminum and silica gel column separation. The amount of chloroform ether used in these methods is relatively large, and the cost is relatively high. In addition, the separation and treatment capacity of silica gel or alumina colu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D219/06
Inventor 杨存
Owner NANJING TONGZE AGRI SCI & TECH
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