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Preparation method of 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate comparison product

A technology of malate and isobutyl, applied in the field of preparation of 1,4-di[4-(glucose oxygen) benzyl]-2-isobutyl malate reference substance, can solve problems such as inappropriate , to achieve the effect of strong specificity, low separation cost and large amount of preparation

Inactive Publication Date: 2010-10-20
BEIJING UNIV OF TECH
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Problems solved by technology

However, this method is a systematic separation of white and chemical components, and is not suitable for the separation and preparation of 1,4-bis[4-(glucose oxygen)benzyl]-2-isobutyl malate
And for 1,4-bis[4-(glucose oxygen) benzyl]-2-isobutyl malate is separated the method that there is no bibliographical information yet

Method used

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  • Preparation method of 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate comparison product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Pulverize the white and medicinal materials into coarse powder, according to the weight ratio of white and coarse powder: 80% ethanol = 1: 12, reflux extraction for 2 hours, and recover the solvent from the filtrate to obtain the liquid extract;

[0025] (2) Dilute the above-mentioned Baiji liquid extract with water at a weight ratio of 1:6, enrich the diluted solution with D101 macroporous adsorption resin, elute with 70% ethanol, collect the eluate, recycle the solvent, and obtain a concentrated solution , add silica gel and mix evenly, the amount of silica gel added is based on white and coarse powder: silica gel=1: 0.05 (weight), and dry at room temperature to obtain dry powder;

[0026] (3) Transfer the above-mentioned dry powder into a chromatographic column, and use chloroform:methanol=1:0, 1:0.3, 1:0.6 as the eluent to elute successively, collect the eluent successively, and detect it by thin-layer chromatography. Recognize, combine 1,4-bis[4-(glucose oxygen...

Embodiment 2

[0030] (1) Pulverize the white and medicinal materials into coarse powder, according to the weight ratio of white and coarse powder: 60% ethanol = 1: 8, reflux extraction for 4 hours, recover the solvent from the filtrate, and obtain the liquid extract;

[0031] (2) Dilute the above-mentioned Baiji liquid extract with water at a weight ratio of 1:8, enrich the diluted solution through AB-8 macroporous adsorption resin, elute with 50% ethanol, collect the eluate, recycle the solvent, and obtain Concentrate, add silica gel and mix evenly, the amount of silica gel added is based on white and coarse powder: silica gel = 1: 0.1 (weight), dry at room temperature to obtain dry powder;

[0032] (3) Transfer the above-mentioned dry powder into a chromatographic column, and use chloroform:methanol=1:0.1, 1:0.3, 1:0.7 as the eluent to elute successively, collect the eluents successively, and detect them by thin-layer chromatography. Recognize, combine 1,4-bis[4-(glucose oxygen) benzyl]-2...

Embodiment 3

[0036] (1) Pulverize the white and medicinal materials into coarse powder, according to the weight ratio of white and coarse powder: 30% methanol = 1: 16, reflux extraction for 6 hours, recover the solvent from the filtrate, and obtain the liquid extract;

[0037] (2) Dilute the above-mentioned Baiji fluid extract with water at a weight ratio of 1:10, enrich the diluted solution through AB-8 macroporous adsorption resin, elute with 40% ethanol, collect the eluate, recycle the solvent, and obtain The concentrated solution is mixed with silica gel evenly, the amount of silica gel added is based on white and coarse powder: silica gel = 1: 0.08 (weight), and dried at room temperature to obtain a dry powder;

[0038](3) Transfer the above-mentioned dry powder into a chromatographic column, and use chloroform:methanol=1:0.1, 1:0.4, 1:0.9 as the eluent to elute successively, collect the eluent successively, and detect it by thin-layer chromatography. Recognize, combine 1,4-bis[4-(glu...

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Abstract

The invention relates to a preparation method of a 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate comparison product. The method comprises the following steps of: pulverizing a rhizoma bletillae medicinal material into coarse powder, extracting in alcohol and recovering the alcohol; adding water to an obtained concentrated solution to dilute and enriching through a macroporous adsorption resincolumn; hydrolyzing and adsorbing in alcohol, and recovering the alcohol to obtain a concentrated solution; adding silica gel to the concentrated solution and uniformly mixing; drying to form powder and eluting by using chloroform and methanol to obtain a crude 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate product; carrying out gel column chromatography to obtain a fine 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate product; and then carrying out preparative reverse silica gel column chromatography and methanol-water elution to obtain the 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate comparison product. Detected by using a high efficiency liquid chromatography method, the content of the 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate can reach higher than 98 percent. The method has lower cost, simple step and strong specificity.

Description

technical field [0001] The invention relates to a preparation method for extracting and separating 1,4-bis[4-(glucose-oxy)benzyl]-2-isobutylmalate reference substance from the traditional Chinese medicine Baiji. technical background [0002] The traditional Chinese medicine Baiji is the dry tuber of Orchidaceae Baiji and Bletilla striata (Thunb.) Reichb.F. It tastes bitter, sweet, astringent, and slightly cold in nature. Baiji is not only commonly used in traditional Chinese medicine, but also widely used in food additives and cosmetics. [0003] In view of the lack of reference substances, even in the newly promulgated 2010 edition of the "Chinese Pharmacopoeia", there are only traits, identification and inspection items under the quality control item of Baiji, lack of content determination of relevant index components, and it is difficult to accurately control its internal quality. In the study of the traditional Chinese medicine Baiji, it was found that the content of 1,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 李霄李泽琳艾萍孙媛媛王小利
Owner BEIJING UNIV OF TECH
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