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Preparation method of acacetin

A technology of locustine and ethanol, applied in the direction of organic chemistry, can solve the problems of cumbersome steps, complicated operation, high cost, etc., and achieve the effect of short steps, high purity and simple method

Inactive Publication Date: 2017-06-16
石河子大学医学院第一附属医院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Invention patents such as Wang Xiumin (the method for separating and preparing acacia monomer from wild chrysanthemum: CN, CN 103193748A[P].) adopt techniques such as extraction, macroporous resin column chromatography, hydrolysis, high-speed countercurrent chromatography to extract from 1kg of wild chrysanthemum plant 10 mg of locust was obtained by separation, and the process adopted 5 kinds of technologies for separation, the operation was complicated, the cost was high, and the yield was low
[0010] Bian Yuping's invention patent (a method of extracting acacia from chrysanthemum: CN, CN 102491964 A[P].) adopts techniques such as extraction, macroporous resin, polyamide column chromatography and recrystallization from 10kg of chrysanthemum plants 1.2g of locust was isolated, the operation was complicated and the steps were cumbersome
[0011] The invention patent of Liu Xiaoqiu et al. (a kind of preparation method and application CN of flavonoids and total flavonoids thereof, CN101475619 A[P].) adopts reflux extraction, macroporous resin, polyamide column chromatography, silica gel column chromatography and SephadexLH -20 column chromatography and other techniques to separate locustine, this process adopts 5 kinds of techniques to separate, the operation is complicated and the steps are cumbersome

Method used

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  • Preparation method of acacetin
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preparation example Construction

[0030] The preparation method of acaciacin provided by the present invention comprises the steps of obtaining the extract of Cinnamon chinensis, further purifying the extract, chromatography, crystallization and the like. The method provided by the present invention will be described in detail below in conjunction with the accompanying drawings.

[0031] like figure 1 As shown, at first, the dried aerial parts of 1 part of fennel are pulverized, extracted with 40-95 vol% alcohol solution of 15-25 times by weight, for example, ethanol or methanol or propanol or any mixture thereof can be used for infiltration. Roll extraction 1-2 times, each extraction 6-24h. Then, the extract is concentrated, for example, the method of concentrating under reduced pressure can be used, and the extract is in the form of paste after concentration. Then the paste is dried, for example, the paste can be made into extract powder by vacuum drying.

[0032] Purify the extract powder with alcohol so...

Embodiment 1

[0039] Embodiment 1: extract and isolate the method that obtains acaciacetin from sweet blue orchid, carry out according to the following steps:

[0040] a. Crush the dried aboveground part of Cymbidium, soak in 10 times the amount of 40% ethanol for 24 hours;

[0041] b. Using the percolation method, the ratio of 3.6kg of Chinese orchid medicinal material to 75% ethanol is 1:40, and the flow rate is 6mL / min, and the ethanol percolation liquid is collected;

[0042] c, the percolate is filtered twice with a mesh with an aperture of 0.5mm, and the filtrates are combined;

[0043] d. Using a vacuum distillation device, at a pressure of 0.08Mpa and a temperature of 30-60°C, distill and remove ethanol to obtain a thick extract of 1.2g / mL; after drying in a water bath, 500g of extract powder is obtained;

[0044] e. Dissolve 100g of extract powder in 70% ethanol and dry mix the sample, apply 100-200 mesh polyamide for column chromatography, and use 40-95% ethanol gradient elution to...

Embodiment 2

[0056] Embodiment 2: extract and isolate the method that obtains acaciacetin from sweet blue orchid, carry out according to the following steps:

[0057] a. Crush the dried aboveground part of the orchid and soak it with 10 times the amount of 75% ethanol for 18 hours;

[0058] b. Using the percolation method, the ratio of 3.0kg of Chinese herbal medicine and 75% ethanol is 1:35, the flow rate is 6mL / min, and the ethanol percolation liquid is collected;

[0059] c. The percolate is filtered once with a mesh with a pore size of 0.1 mm, and the filtrates are combined;

[0060] d. Using a vacuum distillation device, at a pressure of 0.09Mpa and a temperature of 60°C, distill off ethanol to obtain a thick extract of 1.0g / mL; after drying in a water bath, 410g of extract powder is obtained;

[0061] e. Dissolve 100g of extract powder in 70% ethanol and dry mix the sample, apply 100-200 mesh polyamide for column chromatography, use 40-75% ethanol gradient elution to obtain a total ...

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Abstract

The invention relates to a method for extracting and separating acacetin from Dracocephalum moldavica L.. The method comprises the following steps: crushing the dry overground part of Dracocephalum moldavica L., carrying out collection and extraction by using a percolation process to obtain a percolation liquid, and concentrating the percolation liquid through a reduced pressure distillation device to obtain thick extract; carrying out water bath drying on the thick extract to obtain extract powder; dissolving the extract powder in high-concentration alcohol, carrying out dry stirring, carrying out polyamide column chromatography, carrying out elution, and evaporating the obtained eluate by the reduced pressure distillation device until the eluate is dry in order to obtain extract powder; and re-crystallizing the extract powder, and evaporating obtained crystals through the reduced pressure distillation device until the crystals are dry in order to obtain pale yellow crystals which are the compound acacetin.

Description

technical field [0001] The invention relates to a method for extracting and isolating acaciacetin from sweet green orchid. Background technique [0002] According to the literature search, there are some literature reports on the extraction method of locustin: [0003] Chen Zhengxiong (Research on the flavonoids of traditional Chinese medicine VIII. Research on the components of wild chrysanthemum (the first report) [J]. Acta Pharmaceutica Sinica, 1962 (06).) reported for the first time the structure of locustin isolated from wild chrysanthemum. , recrystallization, hydrolysis and other technologies combined to separate acacia from Chrysanthemum chrysanthemum, the operation is complex, the steps are cumbersome and the yield is low. [0004] The structural formula of locust is: [0005] [0006] Chen Weijia (Study on the chemical constituents of wild chrysanthemum and the extraction process of total flavonoids [D]. Shandong University of Traditional Chinese Medicine, 200...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40
Inventor 王新春袁勇邢建国王晓义刘杨黄川生赵洁焦胜春
Owner 石河子大学医学院第一附属医院
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