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Method for preparing hypericins

A hypericin and water extraction technology, applied in organic chemistry, quinone separation/purification, etc., can solve problems such as unfavorable large-scale production, difficult product extraction, troublesome extraction agent configuration, etc.

Inactive Publication Date: 2010-06-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The extraction of hypericin usually uses ethanol, yet because the content of hypericin in Hypericum perforatum is still quite low (0.01~0.06%), it is difficult to extract the product, the yield and purity are not high and the cost is high
As in the method disclosed in Chinese patent CN1880328, hypericin is obtained by macroporous resin adsorption and reverse micellar extraction agent extraction, and the extraction agent configuration is troublesome, which is not conducive to large-scale production; and as the Chinese patent CN1392130 alcohol extraction operation has many repetitions, The end point is not easy to judge

Method used

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  • Method for preparing hypericins

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Grind 20kg of fresh Hypericum perforatum (hypericin content 0.028%), add 200L saturated lime water to soak, heat to 40°C and stir for 1 hour, filter while hot, cool the filtrate to room temperature, add hydrochloric acid to adjust the pH to 6.1; the above solution is passed through the column The SA-5B resin column with a volume of 5L is used for saturated adsorption, and the resin is eluted with 40L water and a sufficient amount of 40% ethanol solution until the effluent is transparent, and then the hypericin eluate is eluted with 50L pure ethanol, and concentrated under reduced pressure; The obtained extract was mixed with neutral alumina and put on the column, eluted with 30% ethanol until the effluent was transparent, eluted twice with 70% ethanol until the effluent was transparent, and concentrated the second eluate to the original volume under reduced pressure 1 / 10, standing to crystallize; the crystals were recrystallized three times with cyclohexane to finally ob...

Embodiment 2

[0030] Grind 20kg of fresh Hypericum perforatum (0.031% hypericin content), add 220L of saturated lime water, soak and heat to 45°C and stir for 1.5 hours, filter while hot, cool the filtrate to room temperature, add hydrochloric acid to adjust the pH to 6.6; the above solution is passed through the column The HPD600 macroporous resin column with a volume of 5L is used for saturated adsorption, and the resin is eluted with 45L of water and a sufficient amount of 50% ethanol solution until the effluent is transparent, and then the hypericin eluate is eluted with 70L of 90% ethanol, and concentrated under reduced pressure; The obtained extract was mixed with neutral alumina and put on the column, eluted with 35% ethanol until the effluent was transparent, eluted twice with 80% ethanol until the effluent was transparent, and concentrated the second eluate to the original volume under reduced pressure 1 / 11, standing for crystallization; the crystals were recrystallized 4 times with...

Embodiment 3

[0032] Grind 20kg of fresh Hypericum perforatum (hypericin content 0.030%), add 240L saturated lime water to soak, heat to 50°C and stir for 2 hours, filter while hot, cool the filtrate to room temperature, add hydrochloric acid to adjust the pH to 7; the above solution is passed through the column The HZ-841 macroporous resin column with a volume of 5L is used for saturated adsorption, and the resin is eluted with 50L water and a sufficient amount of 60% ethanol solution until the effluent is transparent, and then the hypericin eluate is eluted with 75L 80% ethanol, and the eluent is decompressed. Concentrate; the obtained extract is mixed with neutral alumina and put on the column, eluted with 40% ethanol until the effluent is transparent, eluted twice with 90% ethanol until the effluent is transparent, and the second eluent is concentrated under reduced pressure to The original volume was 1 / 12, and it was crystallized upon standing; the crystal was recrystallized five times ...

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Abstract

The invention relates to a method for separating and purifying hypericins by adopting a macroporous resin separation technique and an alumina chromatographic technique. The method comprises the following steps of: grinding fresh hypericum perforatum L, leaching the ground hypericum perforatum L for 1 to 2 hours in saturated lime solution, adjusting a pH value to 6 to 7 by hydrochloric acid at normal temperature, and performing resin separation, segmented elution, alumina chromatography, ethanol elution and cyclohexane to obtain the finished product. The method has the advantages of simple process, little energy consumption and high-purity hypericins.

Description

Technical field: [0001] The invention relates to a process for extracting and purifying hypericin, in particular to a method for purifying hypericin by using resin adsorption and alumina chromatography. Background technique: [0002] Hypericin [0003] Chemical name: 4,4',5,5',7,7'-hexahydroxy-2,2'-dimethyl-medium benzodianthrone (4,4',5,5',7, 7'-Hexahydroxy-2, 2'-dimethyl-naphthodianthrone) [0004] Molecular formula: C 30 h 16 o 8 [0005] [0006] Molecular weight: 504.43 [0007] Properties: blue-black needle-like crystal (pyridine-methanol containing HCl), melting point 320°C (decomposition), easily soluble in pyridine or other organic amines with orange-red fluorescence, insoluble in most organic solvents, soluble in alkaline aqueous solution. It is unstable to light, oxygen and heat. [0008] Hypericin is the main active ingredient of Hypericum perforatum. It has anti-virus, anti-cancer, anti-depression and other functions. It has been used to treat depres...

Claims

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Application Information

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IPC IPC(8): C07C50/36C07C46/10
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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