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Method for preparing high-purity 8-acetyl Shanzhiside methyl ester

A technology of shanzhiside methyl ester and acetyl, which is applied in the field of preparing 8-acetyl shanzhiside methyl ester, can solve the problems of low yield, difficult industrialization and the like, and achieves the effects of safe dissolution, simple process flow and high purity

Inactive Publication Date: 2013-06-05
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this document reports the extraction and separation method of this compound, its yield is extremely low, and 8-acetylshanzhiside methyl ester (4,8-acetyl -shanzhigenin methyl es ter) 12.3 mg
The samples obtained in the research are all at the milligram level, which is difficult to industrialize. In addition, there are also problems in the application of toxic organic solvents in the research process

Method used

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  • Method for preparing high-purity 8-acetyl Shanzhiside methyl ester
  • Method for preparing high-purity 8-acetyl Shanzhiside methyl ester
  • Method for preparing high-purity 8-acetyl Shanzhiside methyl ester

Examples

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Embodiment 1

[0036] Take 1 kg of dry and crushed four-lens hemp of 60 mesh, add 15 kg of 60% ethanol and soak and extract at a temperature of 50°C for 10 hours, add 60% ethanol to the residue and soak and extract at a temperature of 50°C for 8 hours, repeat Extracted three times, combined the extracts, and recovered ethanol under reduced pressure to obtain 134 g of extract. Fully dissolve the extract with ethyl acetate / ethanol mixed solvent (volume ratio: 2:5), filter off the insoluble matter, and use a mixture of silica gel and diatomaceous earth (mass ratio: 1:3) with a mass multiple of 3 times for the filtrate Mix the sample, place the mixed sample in a ventilated place to dry, and pass through a 100-mesh sieve; place the sieved sample in a 2000 ml Erlenmeyer flask, add ethyl acetate, ethyl acetate-ethanol (4:1, 3:1 , 2:1), extracted with ethanol respectively, each time the solvent was 3 times the weight of the mixed sample, and the extraction times were 2 times. The ethyl acetate-etha...

Embodiment 2

[0040]Take 3 kg of dry and crushed 60-mesh four-lens hemp, add 30 kg of 60% ethanol, soak and extract at a temperature of 50°C for 10 hours, add 60% ethanol to the residue, and soak and extract at a temperature of 50°C After 8 hours, the extraction was repeated three times, the extracts were combined, and ethanol was recovered under reduced pressure to obtain 452 g of extract. Fully dissolve the extract with ethyl acetate / ethanol mixed solvent (volume ratio: 2:5), filter off the insoluble matter, and use a mixture of silica gel and diatomaceous earth (mass ratio: 1:3) with a mass multiple of 3 times for the filtrate Mix the sample, place the mixed sample in a ventilated place to dry, and pass through a 100-mesh sieve; place the sieved sample in a 2000 ml Erlenmeyer flask, add ethyl acetate, ethyl acetate-ethanol (4:1, 3:1 , 2:1), extracted with ethanol respectively, each time the solvent was 3 times the weight of the mixed sample, and the extraction times were 2 times. The et...

Embodiment 3

[0044] Take 5 kg of dried and crushed 60-mesh four-lens hemp, add 80 kg of 60% ethanol, soak and extract at a temperature of 60°C for 10 hours, add 60% ethanol to the residue, and soak and extract at a temperature of 60°C After 8 hours, the extraction was repeated three times, the extracts were combined, and ethanol was recovered under reduced pressure to obtain 741 g of extract. Fully dissolve the extract with ethyl acetate / ethanol mixed solvent (volume ratio: 2:5), filter off the insoluble matter, and use a mixture of silica gel and diatomaceous earth (mass ratio: 1:3) with a mass multiple of 3. Mix the sample, place the mixed sample in a ventilated place to dry, and pass through a 100-mesh sieve; place the sieved sample in five 2000 ml Erlenmeyer flasks, add ethyl acetate, ethyl acetate-ethanol (4:1,3 : 1, 2: 1), extracted with ethanol respectively, each time the solvent was 3 times the weight of the mixed sample, and the extraction times were 2 times. The ethyl acetate-et...

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Abstract

The invention relates to a method for preparing high-purity 8- acetyl Shanzhiside methyl ester. According to the method for the preparing high-purity 8-acetyl Shanzhiside methyl ester, phlomis umbrosa roots are adopted as raw materials, dried roots (four stare blankly hemp in Tujia medicine) are extracted through labiatae phlomis umbrosa 40%-60% (V / V) ethanol after the phlomis umbrosa is smashed, extraction separation methods, such as solvent extraction, solid-liquid extraction, reverse phase silica gel column chromatography and gel column column chromatography separation, are carried out, and the 8-acetyl Shanzhiside methyl ester is prepared and separated from the four stare blankly hemp. The method for the preparing high-purity 8- acetyl Shanzhiside methyl ester is simple, and fast. 8-acetyl Shanzhiside methyl ester products obtained with the method is high are purity, high in yield, can capable of laying foundation for development and research in the future.

Description

technical field [0001] The present invention relates to a method for preparing high-purity iridoid glycoside compound 8-acetylshanzhiside methyl ester from the folk medicine Rhizoma Rhizoma Rhizoma, especially a method of ethanol extraction, solid-liquid extraction, and reversed-phase silica gel column layer A method for preparing 8-acetyl shanzhiside methyl ester through analysis and gel column separation and decolorization. Background technique [0002] 8-O-acetylshanzhiside methyl ester is an iridoid glycoside compound. [0003] English name: 8-O-Acetyl shanzhiside methyl ester [0004] Molecular weight: 448 [0005] Molecular formula: C 19 h 28 o 12 [0006] Structural formula: [0007] [0008] 8-O-acetylshanzhiside methyl ester, light yellow amorphous powder, UV 365 Under the strong UV absorption. [0009] The Tujia folk medicine Silenma is the root of the genus Phlomis umbrosa Turcz in the Labiatae family, and the southwestern part of Hubei is the main dis...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 刘普邓瑞雪李军波尹卫平柴元武孙鲜明
Owner HENAN UNIV OF SCI & TECH
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