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Method for extracting calanolide B

A technology of lactone and wool, which is applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems that have not yet been reported on the production process of calatolide B, and achieve easy large-scale production, short time consumption, and short production cycle short effect

Inactive Publication Date: 2013-12-18
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no report on the production process for preparing calanolide B

Method used

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  • Method for extracting calanolide B

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Take the fruit of Hutong tomentosa as raw material, put it into a high-speed tissue grinder, keep it at a speed of 18,000rpm for 5min, pass it through a 40-mesh sieve for later use, weigh 1kg, and use a material-to-liquid ratio of 1:10 (g / ml) After adding 85% ethanol aqueous solution, 0.3% cellulase was added, and the enzymolysis was carried out at 600W ultrasonic power and 48°C for 50 minutes to obtain the enzymatic hydrolysis raw material, which was added to the flash extractor, the extraction voltage was 160V, and the extraction time was For 8 minutes, carry out flash extraction, filter to obtain the extract, concentrate and dry the extract to obtain the crude extract, dissolve it in methanol, dry load the sample to high-pressure silica gel (silica gel mesh number is 200 mesh) column chromatography for purification, and the pressure resistance is 35MPa , the inner diameter of the column is 250mm, the diameter-to-height ratio of the chromatographic column is 1:10, and ...

Embodiment 2

[0025] Take the fruit of Hutong tomentosa as raw material, put it into a high-speed tissue masher, keep it at a speed of 18,000rpm for 3 minutes, pass it through a 40-mesh sieve for later use, weigh 1kg, and use a material-to-liquid ratio of 1:12 (g / ml) After adding 85% ethanol aqueous solution, then add 0.3% cellulase, and enzymolyze for 40min under the conditions of ultrasonic power 600W, 48℃, to obtain the enzymolysis raw material, put it into the flash extractor, the extraction voltage is 160V, the extraction time For 5 minutes, perform flash extraction, filter to obtain the extract, concentrate and dry the extract to obtain the crude extract, dissolve it in methanol, dry load the sample to high-pressure silica gel (silica gel mesh is 200 mesh) column chromatography for purification, and the pressure resistance is 35MPa , the inner diameter of the column is 250mm, the diameter-to-height ratio of the chromatographic column is 1:10, and the gradient elution of chloroform-meth...

Embodiment 3

[0027] Take the fruit of E. chinensis as raw material, put it into a high-speed tissue grinder, keep it at a speed of 18,000rpm for 5 minutes, pass it through a 40-mesh sieve for later use, weigh 1kg, and use a material-to-liquid ratio of 1:15 (g / ml) After adding 85% ethanol aqueous solution, then add 0.3% cellulase, and enzymolyze for 45min under the condition of ultrasonic power 600W, 48℃, to obtain the enzymolysis raw material, put it into the flash extractor, the extraction voltage is 160V, the extraction time For 10 minutes, perform flash extraction, filter to obtain the extract, concentrate and dry the extract to obtain the crude extract, dissolve it in methanol, dry load the sample to high-pressure silica gel (silica gel mesh is 200 mesh) column chromatography for purification, and the pressure resistance is 35MPa , the inner diameter of the column is 250mm, the diameter-to-height ratio of the chromatographic column is 1:10, and the chloroform-methanol is gradient eluted...

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Abstract

The invention discloses a method for extracting calanolide B. The method is characterized by comprising the following steps: using fruits of calophyllum lanigerum var.austrocoriaceum(T.C.Whitmore)P.F.Stevens as raw materials, obtaining raw materials for enzymolysis through tissue breakage and enzymolysis with cellulase, adding the raw materials for enzymolysis to a flash extractor to undergo flash extraction, obtaining an extracting solution through filtration, concentrating and drying the extracting solution, then utilizing high-pressure silica gel column chromatography for purification, collecting fractions of calanolide B, carrying out vacuum concentration, and obtaining calanolide B through supercritical CO2 anti-solvent crystallization. The method disclosed by the invention is simple to operate, is suitable for large-scale production, has the advantages of low energy consumption, low pollution and short production period, and is an environment-friendly production process.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine chemistry, and relates to a method for extracting calatolide B. Background technique [0002] Calanolide B (Calanolide B), the molecular formula is C 22 h 26 o 5 , the molecular weight is 370.45, and the structural formula is [0003] [0004] Calanolide B is a coumarin compound isolated from the fruit of Calophyllum lanigerum var.austrocoriaceum (T.C.Whitmore) P.F.Stevens in the family Guttiferae. Pharmacological studies have shown that calatolide B has anti-HIV-1 effect, and at a concentration of 0.1-10 μM, it has 100% protective effect on HIV-1-infected cells, and can inhibit the replication of HIV-1, and its EC50 is 0.4 μM , IC50 is 15μM, therapeutic index is 37; selectively inhibit HIV-1 reverse transcriptase. [0005] In the prior art, there is no report on the production process for preparing calanolide B. Contents of the invention [0006] The object of the ...

Claims

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Application Information

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IPC IPC(8): C07D493/14
CPCY02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV