Method for separating and purifying diosmetin

A technology for separation and purification of diosmin, which is applied in the fields of organic chemistry and bulk chemical production, can solve the problems such as the lack of industrial production process reports of diosmin, and achieve the advantages of large-scale production operations, low energy consumption, and low pollution Effect

Inactive Publication Date: 2012-01-04
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no industrialized production process report of diosminin

Method used

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  • Method for separating and purifying diosmetin

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Effect test

Embodiment 1

[0018] Take 20kg of whole peppermint from which volatile oil has been extracted, and put in supercritical CO 2 In the extraction kettle, the extraction pressure is 24MPa, the temperature is 35℃, and CO 2 The flow rate is 2mg / g crude drug·min, and the extraction time is 100min. The extract is obtained, dissolved in water, adsorbed by HPD600 macroporous adsorption resin column, eluted with 65% ethanol, collected 5 times the column volume of the eluent, and recovered under reduced pressure. Obtain the concentrated solution, add oxalic acid to adjust the pH to 4.5, use a 10:3 ethyl acetate-methanol mixed solvent to perform 10-stage countercurrent extraction, combine the extracts, recover the solvent under reduced pressure, refrigerate crystallization, add methanol for recrystallization, and separate Crystallize, wash and dry to obtain 4.52g of yellow crystals. After IR, MS, 2 HNMR, 13 CNMR analysis showed that it was geraniol, and its purity was 95.7% by HPLC method.

Embodiment 2

[0020] Take 20kg of the whole peppermint plant from which volatile oil has been extracted, and put in supercritical CO 2 In the extraction kettle, the extraction pressure is 21MPa, the temperature is 40℃, and CO 2 The flow rate is 3mg / g crude drug·min, and the extraction time is 150min. The extract is obtained, dissolved in water, adsorbed by D130 macroporous adsorption resin column, eluted with 55% ethanol, collected 6 times the column volume of the eluent, and recovered under reduced pressure. Obtain the concentrated solution, add dilute hydrochloric acid to adjust the pH to 5.5, perform 8-stage countercurrent extraction with a 10:1 ethyl acetate-water mixed solvent, combine the extracts, recover the solvent under reduced pressure, crystallize in cold storage, and add methanol for recrystallization. The crystals are separated, washed and dried to obtain 4.26g of yellow crystals. After IR, MS, 2 HNMR, 13 CNMR analysis showed that it was geraniol, and its purity was 96.3% by HPLC...

Embodiment 3

[0022] Take 20kg of the whole peppermint plant from which volatile oil has been extracted, and put in supercritical CO 2 In the extraction kettle, the extraction pressure is 29MPa, the temperature is 38℃, and CO 2 The flow rate is 1mg / g crude drug·min, the extraction time is 90min, the extract is obtained, dissolved in water, adsorbed by the NKA-2 macroporous adsorption resin column, eluted with 60% ethanol, collected 3 times the column volume of the eluent, and reduced pressure Recover to obtain the concentrated solution, add dilute phosphoric acid to adjust the pH to 5.0, perform 5-stage countercurrent extraction with a 10:5 ethyl acetate-ethanol mixed solvent, combine the extracts, recover the solvent under reduced pressure, refrigerate and crystallize, add methanol to weight Crystallize, separate the crystals, wash and dry to obtain 4.33g yellow crystals. After IR, MS, 2 HNMR, 13 CNMR analysis showed that it was geraniol, and its purity was 92.4% by HPLC method.

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Abstract

The invention discloses a method for separating and purifying diosmetin. The method comprises the following steps of: taking peppermint pyrrosia petiolosa, from which volatile oil is extracted, as a raw material; adding the peppermint pyrrosia petiolosa into a CO2 supercritical extraction tank to extract; obtaining extract; adsorbing the extract by using aqueous solution through macro-porous adsorption resin; eluting an alcohol-water solution; collecting eluent; decompressing; concentrating; carrying out level reflux extraction on a concentrated solution by using a mixed solvent; mixing extraction solutions; decompressing and recovering the solvent; adding; crystallizing; and drying. The diosmetin is separated and purified by using the method disclosed by the invention. The industrial scale is easy realized. The content of the product is high.

Description

Technical field [0001] The invention belongs to the technical field of traditional Chinese medicine extraction and relates to a method for separating and purifying geraniol. Background technique [0002] Diosmetin, the molecular formula is C 16 H 12 O 6 ; The molecular weight is 300.26, the CAS registration number is 520-34-3, and the melting point is 253-255°C; mainly exists in mint, a plant of the Lamiaceae Mentha haplocalyx In Briq. and other plants, the structural formula is: [0003] [0004] Modern research shows that geraniol has anti-oxidation, anti-infection, anti-shock, anti-mutagenic and anti-allergic properties. [0005] In the prior art, there is no report on the industrial production process of geraniol. Summary of the invention [0006] The technical problem to be solved by the present invention is to provide a method for separating and purifying geraniol which is beneficial to large-scale production operations and has high product purity. [0007] To solve the above ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
CPCY02P20/54
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH
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