Preparation method of hypericum perforatum extractive

A technology for extracting Hypericum perforatum, which is applied in the field of extracting active ingredients of plants, can solve the problems of long extraction time, high instrument cost, and low extraction efficiency, and achieve the effect of saving extraction time and space

Inactive Publication Date: 2011-02-02
ZHEJIANG UNIV CITY COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Extraction method is currently the most widely used method with the lowest cost, but its extraction time is long and the extraction efficiency is low
Carbon dioxide supercritical fluid extraction is currently a relatively advanced extraction method, and the product obtained is also of high purity. After extracting Hypericum perforatum with carbon dioxide supercritical fluid, and then repeatedly extracting with methanol and n-hexane, the obtained extract contains 70% of Hypericin perforatum, but the instrument cost of carbon dioxide supercritical flow extraction method is too high, the yield is low, and it has not been popularized in China

Method used

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  • Preparation method of hypericum perforatum extractive
  • Preparation method of hypericum perforatum extractive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 50 g of the crude extract of Hypericum perforatum, mix it with 250 ml of ethyl acetate, and conduct ultrasonic extraction in an ice-water bath for 60 min. Concentrate the extract obtained above into a concentrated solution containing 0.5-5 g / ml of the crude extract of Hypericum perforatum, adjust the pH to 8 with NaOH, filter with suction, take the filtrate, adjust the pH to 2 with 20% HCl, and use 150 ml of low-boiling petroleum ether Extract 3 to 5 times, combine petroleum ether phases, recover under reduced pressure to obtain extract, and vacuum dry at 0 to 20°C for 2 hours. The above extract was dissolved in a small amount of eluent and subjected to silica gel column chromatography. The eluent was petroleum ether: ethyl acetate: acetic acid = 80:19:1, appropriate amount of pressure was applied, and the collected solution was concentrated to obtain hyperforin-rich Hypericum perforatum extract, detected by HPLC, wherein the content of hypericin is 57%.

Embodiment 2

[0022] Take 50 g of the crude extract of Hypericum perforatum, mix it with 250 ml of ethyl acetate, and perform ultrasonic extraction in an ice-water bath for 30 min. Concentrate the extract obtained above into a concentrated solution containing 0.5-5 g / ml of Hypericum perforatum crude extract, adjust the pH to 8 with NaOH, take the filtrate after low-temperature high-speed centrifugation, adjust the pH to 2 with 20% HCl, and use 150 ml of low-boiling point petroleum Extract with ether for 3-5 times, combine petroleum ether phases, recover under reduced pressure to obtain extract, and dry in vacuum at 0-20°C for 2 hours. Dissolve the above extract in a small amount of eluent and carry out silica gel column chromatography. The eluent is petroleum ether: ethyl acetate = 10:1, pressurize appropriately, and the collected solution is concentrated to obtain a fine extract rich in hyperforin , after detection, wherein the content of hyperforin is 37%.

Embodiment 3

[0024] Take 50 g of the crude extract of Hypericum perforatum and extract it with 250 ml of ethyl acetate for 24 hours. Concentrate the extract obtained above into a concentrated solution containing 0.5-5 g / ml of the crude extract of Hypericum perforatum, adjust the pH to 8 with NaOH, filter with suction, take the filtrate, adjust the pH to 2 with 20% HCl, and use 150 ml of low-boiling petroleum ether Extract 3 to 5 times, combine petroleum ether phases, recover under reduced pressure to obtain extract, and vacuum dry at 0 to 20°C for 2 hours. The above extract was dissolved in a small amount of eluent and subjected to silica gel column chromatography. The eluent was petroleum ether: ethyl acetate: acetic acid = 80:19:1, appropriate pressure was applied, and the collected solution was concentrated to obtain hyperforin-rich The refined extract has been tested, and the content of hyperforin is 36%.

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Abstract

The invention discloses a preparation method of hypericum perforatum extractive which is rich in hyperforin, which comprises the following steps of: taking the hypericum perforatum crude extractive which is sold in the market as the raw material; ultrasonically extracting in the ice water bath; preliminarily removing the impurity by means of two-phase extraction and the like to obtain 11-18% hyperforin-containing extractive; and separating and purifying by means of the silica column chromatography technology to obtain 37-57% hyperforin-containing extractive. The pharmacological test proves that the extractive has the functions of the depression resistant and the learning and memorizing promotion. The preparation method is simple and easy, is suitable for the small-scale preparation required by the pharmacological test and the like, and can save the extracting time and space.

Description

technical field [0001] The invention relates to the field of extraction methods of plant effective components, in particular to a method for preparing a hypericin-rich hypericin-rich hypericin extract from a commercially available Hypericum perforatum crude extract. Background technique [0002] Hypericum perforatum contains a variety of chemical components, mainly including naphthalenedianthones, phloroglucinols, flavonoids, volatile oils, amino acids, phenylpropanes and xanthones. Among them, naphthalene dianthrone, phloroglucinol and flavonoids are considered to be the main active ingredients of Hypericum perforatum. Phloroglucinols mainly include hyperforin and adhyperforin. Hyperforin is a lipophilic component and is extremely unstable to light, heat and oxygen. [0003] The known extraction methods of hypericin mainly include leaching method and carbon dioxide supercritical fluid extraction method. Extraction method is currently the most widely used method with the l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61P25/28A61P25/24A61K36/185
Inventor 刘健翔魏峥曦方吟荃李彦
Owner ZHEJIANG UNIV CITY COLLEGE
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