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Preparation method of Clinodiside A

A technology of cutting off blood flow and saponin, which is applied in the field of natural product separation, can solve the problems of less research on extraction methods and cumbersome operations, and achieve the effects of overcoming the inability to reuse, simple regeneration treatment, and prolonging the life of the resin

Inactive Publication Date: 2012-05-09
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent 200510027812.4 "Extraction method of total saponins of blood flow in traditional Chinese medicine", the disclosed method is to separate and purify total saponins in blood flow by water extraction, alcohol precipitation, resin purification, silica gel column chromatography, etc., the method is cumbersome to operate
However, there are few studies on the extraction methods of the existing high-content Duanxueliu saponin A.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 2Kg of crushed medicinal materials, add 20L of water and heat to 65°C for extraction for 3 hours, filter, add 18L of water to the filter residue, heat to 65°C for 2 hours, filter, add 16L of water to heat to 65°C for extraction After 1 hour, filter, combine the filtrate, add 1.2L of ZTC-II traditional Chinese medicine clarifying agent, let it stand, and pass the centrifugal filtrate through a 1.2L HPD100 macroporous resin column, wash with water until the sugar reaction is negative, and use 4L of 70% The ethanol solution was eluted, the ethanol was recovered under reduced pressure by a rotary evaporator, the eluate was concentrated to a density of 1.2, and then extracted three times with 0.4L water-saturated n-butanol, the extract was concentrated, and 0.3L of LH-20 glucose Glycan gel column (diameter-to-height ratio 10:1), eluted with 35% ethanol solution at a flow rate of 0.2ml / min, monitored by TLC, and concentrated the eluate under reduced pressure to obtain 1.5...

Embodiment 2

[0026] Take 5Kg of crushed herbs, add 60L of water and heat to 65°C for extraction for 3 hours, filter, add 50L of water to the filter residue and heat to 65°C for 3 hours, filter, add 40L of water to the filter residue and heat to 65°C for 2 hours, filter, combine the filtrates, add 3L of ZTC-II type traditional Chinese medicine clarifying agent, let it stand, and the centrifuged filtrate passes through 4L of X-5 type macroporous resin column, washes with water until the sugar reaction is negative, and uses 15L of 75% Elute with ethanol solution, recover ethanol under reduced pressure with a rotary evaporator, concentrate the eluate to a density of 1.1, then extract twice with 1L and 0.8L water-saturated n-butanol, concentrate the extract, and add LH-20 Sephadex The column (diameter-to-height ratio 7:1) was eluted with 30% ethanol solution at a flow rate of 0.1 ml / min, monitored by TLC, and the eluate was concentrated under reduced pressure to obtain 3.4 g of crystals with a c...

Embodiment 3

[0028] Take 5Kg of crushed medicinal materials for cutting blood flow, add 50L of water, heat to 70°C for extraction for 3 hours, filter, add 45L of water to the filter residue, heat to 70°C for extraction for 3 hours, filter, add 40L of water to the filter residue, and heat to Extract at 70°C for 2 hours, filter, combine the filtrate, add 3L of ZTC-II traditional Chinese medicine precipitant, let stand, the filtrate passes through 3L of AB-8 macroporous resin column, wash with water until the sugar reaction is negative, and use 12L of Elute with 70% ethanol solution, recover ethanol under reduced pressure with a rotary evaporator, concentrate the eluate to a density of 1.2, extract the concentrated solution with 1L, 0.8L, and 0.6L water-saturated n-butanol for 3 times, and concentrate the extract under reduced pressure. Add LH-20 Sephadex column (diameter-to-height ratio 8:1), elute with 32% ethanol solution at a flow rate of 0.2ml / min, monitor by TLC, and concentrate to obtai...

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Abstract

The invention provides a preparation method of Clinodiside A, comprising the following technological steps of: crushing clinopodium polycephalum, adding 8-15 times of water, heating up and extracting for 2-3 times, sinking the extract by the addition of a sinking agent, adding a macroporous resin into a filtered solution for adsorption, carrying out elution by an ethanol solution with the concentration of 60-80%, carrying out vacuum concentration on the eluent, extracting for 2-3 times by using water-saturated n-butanol, carrying out vacuum concentration on the extract, letting the concentrate pass through a gel column for chromatographic separation, carrying out elution by using ethanol with the concentration of 30-35%, collecting a lower column liquid, reducing pressure and recovering ethanol, and drying to obtain Clinodiside A. The technology provided by the invention is simple to operate, has good reappearance and is suitable for the preparation of the high-content Clinodiside A product.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, in particular to a method for separating saponin A from blood stream by gel column Background technique: [0002] Duanxueliu is a folk herbal medicine in Anhui Province. It is the dry above-ground part of the labiatae plant Campanula spp. The total saponins of Duanxueliu belong to pentacyclic triterpenoid saponins, which are the main hemostatic components in Duanxueliu. Among them, saponin A is the main representative component, which can be used for gynecological bleeding and other hemorrhagic diseases, enteritis, bacillary dysentery, sores and swollen toxins, snake bites and dog bites. Its pharmacological effects mainly include blood coagulation promotion, vasoconstriction, uterine contraction, direct hemostasis, and antibacterial effect. Clinical application has a good effect on various bleeding disorders, especially gynecological bleeding. Duanxueliu saponin A is the main comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
Inventor 李法庆杨成东刘东锋
Owner 苏州宝泽堂医药科技有限公司
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