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A kind of preparation method of selaginellin N

A methanol and ethanol technology, which is applied in the field of preparation of selaginellinN in Selaginella, can solve unseen problems and achieve the effects of high yield, simple process operation and good repeatability

Inactive Publication Date: 2016-08-31
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction method of this selaginellin N is not seen in the prior art at present

Method used

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  • A kind of preparation method of selaginellin N
  • A kind of preparation method of selaginellin N
  • A kind of preparation method of selaginellin N

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Cut 100 g of dried Selaginella herb into inch segments, add 30% ethanol to reflux and extract three times, add 11 times of the amount each time, each time for 2 hours, combine the extracts, filter to obtain the extracts. Recover the ethanol from the extract and concentrate it to a clear paste with a relative density of 1.20 (60°C), add 5 times the amount of water to suspend, and obtain a suspension. Add the suspension to the chromatographic column with D101 type macroporous adsorption resin as the adsorbent for adsorption. Then the adsorption column was eluted with a mixed solvent gradient of ethanol and water (10:1 ~ 1:1), and the eluate fraction was collected at a volume of 1 / 40 of the total eluent in each part, and the spots were checked by TLC (in the order of Chloroform: Methanol 3:1 is the developer), and the elution fractions of the same brown spots were combined. The combined elution fractions of the same brown spots were recovered to the solvent to obtain a br...

Embodiment 2

[0053] Cut 2 kg of dried Selaginella chinensis into inch sections, add 75% ethanol to reflux and extract three times, add 10 times of the amount each time, each time for 1.5 hours, combine the extracts, filter to obtain the extracts. Recover the ethanol from the extract and concentrate it to a clear paste with a relative density of 1.10 (60°C), add 7 times the amount of water to suspend to obtain a suspension. The suspension was added to the chromatographic column with D101 macroporous adsorption resin as the adsorbent for adsorption. Then the adsorption column was eluted with a mixed solvent gradient of ethanol and water (10:1 ~ 1:1), and the eluate fraction was collected at a volume of 1 / 30 of the total eluent in each part, and the spots were checked by TLC (in the order of Chloroform: Methanol 2:1 is the developer), and the elution fractions of the same brown spots were combined. The combined elution fractions of the same brown spots were recovered to the solvent to obtain...

Embodiment 3

[0055] Cut 30 kg of dried Selaginella herb into inch sections, add 50% ethanol to reflux and extract three times, add 9 times of the amount each time, each time for 1.5 hours, combine the extracts, filter to obtain the extracts. Recover the ethanol from the extract and concentrate it to a clear paste with a relative density of 1.25 (60°C), add 10 times the amount of water to suspend to obtain a suspension. The suspension was added to the chromatographic column with D101 macroporous adsorption resin as the adsorbent for adsorption. Then the adsorption column was eluted with a mixed solvent gradient of ethanol and water (10:1 ~ 1:1), and the eluate fraction was collected with a volume of 1 / 20 of the total eluent in each part, and the spots were checked by TLC (in the order of Chloroform: Methanol 3:1 is the developer), and the elution fractions of the same brown spots were combined. The combined elution fractions of the same brown spots were recovered to the solvent to obtain a...

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Abstract

The invention belongs to the technical field of medicines and provides a preparation method of selaginellin N being more than 95% in content from a traditional Chinese medicine selaginella tamariscina. A structure of the compound is represented as the following formula (I). The selaginellin N is prepared with dried whole herb of Selaginella tamariscina(Beauv.) Spring or Selaginella pulvinata(Hook.et Grev.) Maxim. as an initial raw material, and is prepared through extraction by an organic solvent and / or water and separation through a separation process with combination of macroporous resin adsorption and Sephadex LH-20 adsorption. The preparation method is simple in operations, is good in repeatability, is high in yield and is suitable in industrial production. The selaginellin N is high in purity and the content of the selaginellin N is not less than 95% through detection by HPLC.

Description

Technical field: [0001] The invention relates to a preparation method of selaginellin N in selaginella, and its content should be more than 95% as detected by HPLC. It belongs to the field of extraction, separation and purification of traditional Chinese medicine. Background technique: [0002] The 2005 edition of the Chinese Pharmacopoeia stipulates that Selaginella is the dried whole herb of Selaginella tamariscina (Beauv.) Spring or Selaginella pulvinata (Hook. et Grev.) Maxim. It can be harvested throughout the year, remove fibrous roots and sediment, and dry in the sun. Xin, flat. Return liver, heart channel. Has promoting blood circulation and stimulating menstruation. For amenorrhea dysmenorrhea, abdominal mass in the abdomen, and injury from falls. Selaginella charcoal to stop bleeding. For vomiting blood, metrorrhagia, hematochezia, prolapse of the anus. Selaginella contains a variety of chemical components, such as flavonoids. It has been found that Selagine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/753C07C45/78A61K31/122A61P35/00A61P37/02A61P31/12A61P31/04A61P29/00A61P25/20
Inventor 张国刚
Owner SHENYANG PHARMA UNIVERSITY