A method for preparing gentiopicroside chemical reference substance from Gentiana japonica

A technology of gentiopicroside chemistry and gentipicroside, which is applied in the field of preparation of gentiopicroside chemical reference substance, can solve the problem of unstable gentiopicroside chemical reference substance, large loss, and lack of efficient column separation method And the corresponding detection methods and other issues, to achieve the effect of suitable for large-scale production, high recovery rate, and easy to scale

Inactive Publication Date: 2017-08-15
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above methods all apply silica gel column chromatography and crystallization to varying degrees. Although the pure gentiopicroside with high purity can be obtained, the loss in the separation process is very large; at the same time, there is a lack of efficient column separation methods and corresponding detection. method, the gentiopicroside chemical reference substance with a purity of more than 98% cannot be obtained stably and efficiently

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  • A method for preparing gentiopicroside chemical reference substance from Gentiana japonica
  • A method for preparing gentiopicroside chemical reference substance from Gentiana japonica

Examples

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Effect test

Embodiment 1

[0023] Embodiment 1 A kind of method for preparing gentiopicroside chemical reference substance from Gentiana twisted, comprises the following steps:

[0024] (1) 95% ethanol solution extraction:

[0025] 1 Kg of the whole herb of Gentiana gentamiae was dried in the shade and crushed, then added 10 times the mass of an ethanol solution with a volume concentration of 95%, extracted once at 60°C for 3 hours each time, filtered and combined the filtrate A, and the filtrate A was decompressed Dried to a paste, that is, the alcoholic extract of Gentiana mahua.

[0026] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.09 MPa and a temperature of 50 °C.

[0027] ⑵ Resin column enrichment:

[0028] Dissolve the alcohol extract of Gentiana gentamiae in methanol solution with a volume fraction of 30%, and then separate it through an MCI resin column. Methanol solution and 50% methanol solution were used for step gradient elution, 50% eluate was collected,...

Embodiment 2

[0034] Embodiment 2 A kind of method for preparing gentiopicroside chemical reference substance from Gentiana twisted, comprises the following steps:

[0035] (1) 95% ethanol solution extraction:

[0036] 0.5 Kg of Gentiana japonica whole herb was dried in the shade and crushed, then added 4 times its mass in ethanol solution with a volume concentration of 90%, extracted 3 times at 95°C for 1 hour each time, filtered and combined the filtrate A, and the filtrate A was decompressed Dried to a paste, that is, the alcoholic extract of Gentiana mahua.

[0037] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.06 MPa and a temperature of 70°C.

[0038] ⑵ Resin column enrichment:

[0039] Dissolve the alcoholic extract of Gentiana japonica with 5% volume fraction of methanol solution and then separate it through HP20SS resin column, firstly remove the large polar impurities by eluting with 5 times column volume of aqueous solution, and then use 5 times ...

Embodiment 3

[0045] Embodiment 3 A kind of method for preparing gentiopicroside chemical reference substance from Gentiana twisted, comprises the following steps:

[0046] (1) 95% ethanol solution extraction:

[0047] 2.5 Kg of the whole herb of Gentiana japonica, dried in the shade, crushed, added 8 times its mass in ethanol solution with a volume concentration of 80%, extracted twice at 75°C for 2 hours each time, filtered and combined the filtrate A, and the filtrate A was dried under reduced pressure To the creamy state, the alcoholic extract of Gentiana mahua is obtained.

[0048] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.08 MPa and a temperature of 60 °C.

[0049] ⑵ Resin column enrichment:

[0050] Dissolve the alcohol extract of Gentiana japonica in methanol solution with a volume fraction of 10%, and then separate it through the MCI resin column. Methanol solution and 50% methanol solution were used for step gradient elution, 50% eluate was col...

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Abstract

The present invention relates to a method for preparing gentiopicroside chemical reference substance from Gentiana gentipicroside, the method comprising the following steps: (1) extraction with 95% ethanol solution: drying the whole herb of gentipicroside in the shade, crushing, carrying out alcohol extraction, filtering, and drying to paste , to obtain the alcoholic extract of Gentiana japonica; (2) Resin column enrichment: dissolving the alcoholic extract of Gentiana kinkanii with methanol solution and separating it through a resin column, first eluting with aqueous solution to remove large polar impurities, and then using 30% methanol solution, Step gradient elution with 50% methanol solution, collect 50% of the eluate, and dry the 50% of the eluate under reduced pressure to obtain the crude product of Gentiana japonica; (3) Refined by reverse-phase liquid phase preparative chromatography: after the crude product of Gentiana genus twisted is dissolved in methanol solution , after filtration, reversed-phase liquid phase preparative chromatographic separation, the main chromatographic peak fraction in the preparative chromatogram was collected, and the chromatographic peak fraction was dried under reduced pressure to obtain a white powdery reference substance with a purity greater than 98%. The invention has short separation time, good separation effect and high product purity.

Description

technical field [0001] The invention relates to a method for preparing a chemical reference substance of gentiopicroside, in particular to a method for preparing a chemical reference substance of gentiopicroside from Gentiana japonica. Background technique [0002] Twist Gentiana ( Gentiana straminea Maxim.) belongs to Gentianaceae (Gentianaceae) Gentiana ( Gentiana (Tourn.) L ) Herbal plant, Gentiana twisted has the functions of dispelling wind and dampness, clearing heat and promoting gallbladder, relaxing muscles and relieving pain. Gentiopicroside is an iridoid glycoside compound with a content of about 8% in the whole herb of Gentiana. The 2010 edition of the Chinese Pharmacopoeia has included gentiopicroside as one of the quality control index components of Gentiana and stipulated that The content of the total amount of glycosides and loganinic acid in Gentiana twisting medicinal material should reach more than 2.5%. [0003] At present, the extraction method of g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/08C07H17/04
Inventor 党军张莉王启兰陶燕铎梅丽娟邵赟岳会兰刘增根
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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