Hypericin purifying method

A technology of hypericin and purification method, applied in quinone separation/purification, organic chemistry, etc., can solve the problems of low purity of hypericin, complicated process, and pollution of finished products, and achieve high mechanical strength and good chemical stability , High recovery effect

Inactive Publication Date: 2011-06-01
SHENZHEN POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing separation process of high-purity hypericin, conventional separation media such as macroporous resin, polyamide, and silica gel are mainly used to prepare hypericin. Not high, and a large amount of highly toxic organic solvents need to be used in the production process, which is not environmentally friendly, and it is easy to cause pollution to the finished product

Method used

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Experimental program
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Effect test

Embodiment 1

[0029] Step (1): Weigh 100g of Hypericum perforatum extract, crush it, dissolve it in 600mL of 60% ethanol, and extract it ultrasonically for 30min, add 120mL of 10% gelatin solution, adjust the concentration of ethanol to 80%, let it stand for 10h, concentrate and filter to obtain Goldenseal perforatum Peach extract to remove tanning solution 350mL.

[0030] Step (2): PEK microsphere chromatography: suspend PEK microspheres with distilled water, and install them into a chromatography column with a specification of ?1cm×10cm by gravity sedimentation. After the PEK microspheres settle completely, equilibrate the column bed with 15mL distilled water. Take 8mL of Hypericum perforatum detanning solution prepared in (1), load the sample, and elute 16mL, 24mL, 16mL, 24mL, 48mL, 20mL, 56mL, collect 60% ethanol eluate, concentrate to obtain hypericin crude product, the content of hypericin measured by HPLC is 3.2%.

[0031] Step (3): PDCX microsphere chromatography: suspend PDCX micr...

Embodiment 2

[0034] Step (1): Weigh 100g Hypericum perforatum extract and crush it, dissolve it in 800mL of 60% ethanol solution, and then extract it ultrasonically for 30 minutes, add 200mL of 10% gelatin solution, adjust the ethanol concentration to 80%, let it stand for 10 hours, concentrate and filter it Hypericum leaf extract to remove tanning solution 450mL.

[0035] Step (2): PEK microsphere chromatography: suspend PEK microspheres with distilled water, and install them into a chromatographic column with a size of ?1cm×10cm by gravity sedimentation. After the PEK microspheres settle completely, equilibrate the column bed with 15mL distilled water, Add 6 mL of Hypericum perforatum detanning solution prepared in step (1), and then wash 12 mL, 20 mL, 12 mL, 20 mL, 40mL, 16mL, 42mL, collect 60% ethanol eluent, concentrate to obtain hypericin crude product, the content of hypericin measured by HPLC is 3.1%.

[0036] Step (3): PDCX microsphere chromatography: suspend PDCX microspheres in...

Embodiment 3

[0040] Step (1): Weigh 1000g of Hypericum perforatum extract and crush it, dissolve it with 6000mL of 60% ethanol solution and extract it ultrasonically for 30min, add 1200mL of 10% gelatin solution, adjust the ethanol concentration to 75%, let stand for 10h, filter and concentrate Hypericum leaf extract detanning liquid 2500mL.

[0041] Step (2): PEK microsphere chromatography: suspend PEK microspheres with distilled water, and install them into a chromatographic column with a specification of ?5cm×18cm by gravity sedimentation method. After the PEK microspheres settle completely, equilibrate the column bed with 700mL distilled water. Take 350 mL of Hypericum perforatum extract detanning solution prepared in step (1), load the sample, and wash with water, 10% ethanol solution, 30% ethanol solution, 40% ethanol solution, 60% ethanol solution at a flow rate of 10mL / min 525mL, 700mL, 875mL, 525mL, 1400mL, take the eluate of 60% ethanol solution, concentrate until no alcohol smel...

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Abstract

The invention discloses a hypericin purifying method which comprises the steps of: crushing hypericum perforatum extract, ultrasonically extracting after the crushed hypericum perforatum extract is dissolved in an alcohol solution, adding a gelatin solution to remove tan to obtain a hypericum perforatum extract tan-removing solution; mixing methacrylate type polymer microspheres with distilled water for suspending, transferring into a chromatographic column, carrying out wet-process sampling on the hypericum perforatum extract tan-removing solution, carrying out gradient elution by using a water-alcohol solution system, and concentrating eluent to obtain a crude hypericin product; mixing styrene type polymer microspheres with an acetone solution for suspending, transferring into the chromatographic column, completely dissolving the crude hypericin product with the acetone solution, then carrying out the wet-process sampling, carrying out gradient elution by using the acetone solution, and processing eluent to obtain a fine hypericin product; and mixing reverse-phase silica gel filler with chromatographically pure methanol for suspending, transferring into the chromatographic column, completely dissolving the fine hypericin with the methanol, sampling, eluting with a methanol-disodium hydrogen phosphate buffer solution, mixing the same components after eluent is detected by adopting HPLC (High Performance Liquid Chromatography) to obtain the purified hypericin. The hypericin is separated and purified by using the nano microsphere materials, and the content of the hypericin is above 90 percent.

Description

technical field [0001] The invention relates to a technology for preparing hypericin, in particular to a method for purifying hypericin. Background technique [0002] The content of hypericin in the whole plant of Hypericum perforatum is only a few ten thousandths, and the content of hypericin in the extract of Hypericum perforatum in the market is only about 0.3%. At present, the research on hypericin mainly focuses on its extraction process, but there are few studies on the purification process of high-purity hypericin. In the existing separation process of high-purity hypericin, conventional separation media such as macroporous resin, polyamide, and silica gel are mainly used to prepare hypericin. It is not high, and a large amount of highly toxic organic solvents need to be used in the production process, which is not environmentally friendly, and it is easy to cause pollution to the finished product. Contents of the invention [0003] The technical problem to be sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/36C07C46/10
Inventor 张俊松王晓利王金林
Owner SHENZHEN POLYTECHNIC
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