Method for preparing gentiopicroside chemical reference substances from gentiana straminea maxim

A technology of gentiopicroside chemistry and mahuahuan is applied in the field of preparation of gentiopicroside chemical reference substance, which can solve the problem that the chemical reference substance of gentiopicroside cannot be stabilized, and an efficient column separation method and corresponding detection method are lacking. methods, large losses, etc., to achieve the effects of being suitable for large-scale production, easy to scale, and high recovery rate

Inactive Publication Date: 2015-08-12
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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  • Method for preparing gentiopicroside chemical reference substances from gentiana straminea maxim
  • Method for preparing gentiopicroside chemical reference substances from gentiana straminea maxim

Examples

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Embodiment 1

[0023] Example 1 A method for preparing gentiopicroside chemical reference substance from Gentiana japonica, comprising 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, an...

Embodiment 2

[0034] Example 2 A method for preparing gentiopicroside chemical reference substance from Gentiana japonica, comprising 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 col...

Embodiment 3

[0045] Example 3 A method for preparing gentiopicroside chemical reference substance from Gentiana japonica, comprising 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 alcoholic extract of Gentiana japonica with 10% volume fraction of methanol solution and separate it by MCI resin column, firstly remove the large polar impurities by elution with 3 times column volume of aqueous solution, and then use 3 time...

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Abstract

The invention relates to a method for preparing gentiopicroside chemical reference substances from gentiana straminea maxim. The method includes the following steps: (1), drying gentiana straminea maxim herbs in the shade, smashing the herbs, and performing alcohol extraction, filtration and drying on the smashed herbs to obtain paste, namely gentiana straminea maxim extracts; (2), dissolving the gentiana straminea maxim extracts in methanol solutions before resin column separation, eluting and removing high-polarity impurities by water solutions, performing step gradient elution by 30% of methanol solutions and 50% of methanol solutions, collecting 50% of eluates, and drying the eluates under reduced pressure to obtaine gentiana straminea maxim crude products; (3), dissolving the gentiana straminea maxim crude products in the methanol solutions, collecting main chromatographic peak cut fractions in preparative chromatograms through filtering and inverted liquid phase preparative chromatography separation, and drying the chromatographic peak cut fractions under reduced pressure to obtain the white powdery reference substances with purity larger than 98%. The method has the advantages of 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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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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