A kind of preparation method of jujube seed saponin A reference substance

A technology of jujube seed saponin and reference substance, which is applied in the fields of steroids and organic chemistry, and can solve problems such as difficulty in separating monomers, low content of jujube seed saponin A, and insufficient supply

Active Publication Date: 2020-08-11
上海诗丹德标准技术服务有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there are few domestic literature reports on the separation and purification of jujube seed saponin A. In addition, jujube seed saponin A has been listed as a standard in the 2015 edition of the Pharmacopoeia, and its demand is increasing, and the content of jujube seed saponin A in medicinal materials is very high. Low, it is very difficult to separate the monomer from medicinal materials, and the supply on the market is seriously insufficient. Therefore, it is very necessary to separate and purify the reference substance of jujuboside A from jujube seed, which has wide application value

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  • A kind of preparation method of jujube seed saponin A reference substance
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  • A kind of preparation method of jujube seed saponin A reference substance

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[0049] Preparation method of the present invention

[0050] For realizing above-mentioned purpose of the invention, the technical scheme that the present invention adopts is as follows:

[0051] A kind of preferred technical scheme of the present invention is as follows:

[0052] A. Extraction of raw materials: adding 5 to 8 times the amount of ethanol solution according to the volume and mass ratio L / Kg of the Chinese date seed medicinal material, and the volume percentage concentration of the used ethanol solution is 60-75%; Heat extraction at least 2 times at ℃, about 2 hours each time, cool to room temperature, filter with suction, combine the filtrates, and concentrate until there is no alcohol smell;

[0053] B. macroporous resin enrichment: the concentrated solution of step A is statically adsorbed overnight with macroporous resin, and then use 2-3 times of column volume water and 2-5 times column volume of 15-30% ethanol solution Elute the impurities, and then use 1-...

Embodiment 1

[0066] The preparation method of jujuboside A reference substance, it is carried out according to the following process steps:

[0067] A. Raw material extraction: Add 100Kg of jujube seed medicinal material to 600L ethanol solution with a volume fraction of 70%, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, filter with suction, combine the filtrates, and concentrate to no alcohol Flavor, 30L in total;

[0068] B. Enrichment of macroporous resin: Weigh 20KgD101 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 15 hours overnight, and then use 80L of water and 30% ethanol solution of 50L column volume respectively Elute the impurities, then elute the target substance with 30L of 60% ethanol solution, collect the eluate, and concentrate to 1000ml;

[0069] C. Extraction: Add 2000ml of n-butanol to the concentrated solution of step B, extract, collect th...

Embodiment 2

[0079] A. Raw material extraction: Add 500Kg of Chinese jujube seed medicinal material to 2500L of ethanol solution with a volume fraction of 70%, heat extraction at 60°C for 2 times, each time for 2 hours, cool to room temperature, filter with suction, combine the filtrates, and concentrate to no alcohol Flavor, 150L in total;

[0080] B. Macroporous resin enrichment: Weigh 100KgD101 macroporous adsorption resin and pack it into a column, statically adsorb the concentrated solution of step A with macroporous resin for 20 hours overnight, and then use 400L of water and 30% ethanol solution of 250L column volume respectively Elute the impurities, then elute the target substance with 150L of 60% ethanol solution, collect the eluate, and concentrate to 5000ml;

[0081] C. Extraction: Add 10L n-butanol to the concentrated solution of step B, extract, collect the n-butanol layer, and concentrate to obtain the ethanol extract of jujuboside A described in step (i);

[0082] D. Mediu...

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Abstract

The invention discloses a preparation method of a jujuboside A reference substance. Specifically, the preparation method disclosed by the invention comprises the steps of (i) providing an alcohol extract of jujuboside A; (ii) dissolving the alcohol extract and separating an alcohol extract mixture by using a medium pressure preparative column to obtain a jujuboside A semi-finished product; (Iii) dissolving the jujuboside A semi-finished product and separating by using a gel column to obtain a jujuboside A crude product; (iv) dissolving the jujuboside A crude product, and preparing under high pressure to obtain jujuboside A high pressure fraction; (v) concentrating and freeze-drying the jujuboside A high pressure fraction to obtain the jujuboside A reference substance. The preparation method has the advantages of stable technology, convenient operation, high separation efficiency, low cost, economic and environmental protection effect, higher economic value and higher academic value.

Description

technical field [0001] The invention belongs to the technical field of modernization of traditional Chinese medicine, and relates to a preparation method of a chemical reference substance of traditional Chinese medicine. Specifically, the invention provides a method for separating a high-purity jujube seed saponin A reference substance from wild jujube seed. Background technique [0002] Ziziphi Spinosae Semen is the dry mature seed of Ziziphus jujuba Mill.var.spinosa (Bunge) Huex H.F.Chou, a plant of the genus Ziziphus jujuba in Rhamnaceae. It has the functions of calming the heart, suppressing sweat, and promoting body fluid. It is used for symptoms such as fatigue and insomnia, palpitations and dreaminess, body deficiency and hyperhidrosis, and thirsty wounds. "Compendium of Materia Medica" listed it as the top grade. Suanzaoren has high medicinal value, and its pharmacological effects have been deeply studied. The jujube seed saponin is a relatively high content compone...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
Inventor 钱勇舒亚平辛振强冯宝军何晓义谢天培
Owner 上海诗丹德标准技术服务有限公司
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