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Method for separating benzoxazole oxazinone glycoside compounds from acanthus

A compound and a separation technology are applied in the field of separating benzoxazinone glycoside compounds from rat scorpion, and achieve the effects of less solvent consumption, organic solvent saving and fast separation speed.

Active Publication Date: 2008-12-10
SOUTH CHINA SEA INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no relevant research on the application of high-speed countercurrent chromatography technology to the separation of benzoxazinone compounds in rat bougainvillea.

Method used

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  • Method for separating benzoxazole oxazinone glycoside compounds from acanthus
  • Method for separating benzoxazole oxazinone glycoside compounds from acanthus
  • Method for separating benzoxazole oxazinone glycoside compounds from acanthus

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Dry 1kg of the aboveground part of rat botanicals and pulverize, extract 3 times with volume fraction of 95% ethanol (5000mL) at room temperature, evaporate the extract and suspend it in water, add petroleum ether to extract, separate the organic phase after layering (repeat 3 times) ), add ethyl acetate to the water phase for extraction, after layering, separate the organic phase (repeat 3 times), add n-butanol to the water phase for extraction, separate the organic phase (repeat 3 times), and distill the organic phase under vacuum After the solvent is removed, 40g of the n-butanol extract is obtained and stored at 4°C for later use. The HPLC analysis chromatogram of the n-butanol extract is shown in Figure 4 (1).

[0020] Ethyl acetate, n-butanol and 0.5% ammonia are mixed in a volume ratio of 2:3:5 to obtain a solvent system of 1000 mL. After mixing, the solvent is fully balanced at room temperature, and the two phases are separated before use. A sample of 100 mg of n-bu...

Embodiment 2

[0027] Dry 1kg of the aboveground part of rat botanicals and pulverize, extract 3 times with volume fraction of 95% ethanol (5000mL) at room temperature, evaporate the extract and suspend it in water, add petroleum ether to extract, separate the organic phase after layering (repeat 3 times) ), add ethyl acetate to the water phase for extraction, after layering, separate the organic phase (repeat 3 times), add n-butanol to the water phase for extraction, separate the organic phase (repeat 3 times), and distill the organic phase under vacuum After the solvent is removed, 40g of the n-butanol extract is obtained and stored at 4°C for later use. The HPLC analysis chart of the n-butanol extract is shown in Figure 4 (1).

[0028] The first step: mixing ethyl acetate, n-butanol and water in a volume ratio of 2:3:5 to obtain a solvent system of 10000 mL, the solvent is fully balanced at room temperature after mixing, and the two phases are separated before use. Take a sample of 1600 mg of...

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Abstract

The invention relates to a method for separating a benzoxazine ketone compound (R is H or OH) as shown in a formula (1) from Acanthus ilicifolius L. The method is characterized in that: an upper phase of a solvent system consisting of three compositions a, b and c according to a volume ratio of 2-5 to 3-6 to 5-10; a lower phase of the solvent system is used as a mobile phase, wherein, the composition a is ethyl acetate, propyl acetate or isopropyl acetate; the composition b is normal butanol, isobutyl alcohol or pentanol; the composition c is water or a hartshorn; a normal butanol extractant of the Acanthus ilicifolius L is dissolved in the solvent system to prepare a sample solution; flow fractions are detected by an ultraviolet spectrograph through a high-speed countercurrent chromatography and collected according to a chromatographic peak, and the compound with the formula (1) is obtained, wherein R represents H or OH. The method can save mass organic solvents; a separation process only needs 3 to 6 hours; the produced compound has a purity of over 80 percent; and the product can be directly used for standard chromatograpical samples, pharmacological experiments or business applications.

Description

Technical field [0001] The present invention relates to a method for separating benzoxazolidinone compounds from Acanthus ilicifolius L., in particular to a method for separating the following formula from Acanthus ilicifolius L. using high-speed countercurrent chromatography technology ( 1) (2R)-2-O-β-D-glucosyl-2H-1,4-benzoxazosin-3(4H)-one and (2R)-2-O-β-D- Glucosyl-4-hydroxy-2H-1,4-benzoxazosin-3(4H)-one. Background technique [0002] Rat botanical is a perennial herb, the whole plant can be used as medicine, mainly treating lymphadenitis, hepatitis, asthma and so on. Pharmacological studies have shown that the extract of rat botanical has anti-viral, anti-cancer, anti-oxidant, anti-mutation, hepatoprotective and anti-inflammatory activities. At present, 6 kinds of benzoxazolidinone compounds have been extracted from rat botanicals. Such compounds mainly play the role of resisting pests and diseases in plants, competing with other plants through allelopathy, and growth hormon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08B01D15/34
Inventor 张偲尹浩罗雄明李庆欣
Owner SOUTH CHINA SEA INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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