Extracting and purifying technology for haw flavonoids substances

A technology of hawthorn extract and total flavonoids, applied in medical preparations containing active ingredients, plant/algae/fungus/moss components, plant raw materials, etc., can solve the comprehensive and systematic research on the extraction and purification process of hawthorn total flavonoids that have not been seen, etc. problem, to achieve the effect of shortening the heating time, high transfer rate and preventing clogging

Inactive Publication Date: 2008-01-16
湖北中医学院
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] There are many literatures on the extraction and purification process of total flavonoids from hawthorn leaves, but there is no report on the com...

Method used

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  • Extracting and purifying technology for haw flavonoids substances
  • Extracting and purifying technology for haw flavonoids substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Extraction process experiment of hawthorn total flavonoids

[0029] (1) use the ethanol reflux extraction method to carry out the experiment, adopt L 9 (3 4 ) Orthogonal experimental method to investigate the process parameters of ethanol concentration, ethanol dosage (multiple of hawthorn weight), extraction time and particle size of decoction pieces in ethanol reflux extraction of total flavonoids in hawthorn, and adopt ultraviolet-visible spectrophotometry to analyze the total flavonoids in the extract. The content was measured and used as an index for comparative analysis. The results are shown in Table 1, Table 2 and Table 3.

[0030] Table 1 Level table of experimental factors

[0031]

Level

factor

A

Ethanol concentration (%)

B

Ethanol consumption (multiple)

C

time (hours)

D.

Particle size

1

2

3

60

70

80

...

Embodiment 2

[0039] Example 2 Macroporous resin purification process experiment of hawthorn total flavonoids

[0040] The hawthorn extract that extracts with aforementioned optimal extraction condition is carried out following experiment:

[0041] (1) Screening experiment of macroporous resin

[0042] Resin source: D101 resin (Tianjin Haiguang Chemical Co., Ltd.), AB-8, D4020 resin (Nankai University Chemical Plant), SP825, HP20, SP70 (Japan Mitsubishi Corporation).

[0043] The screening results of the resin are shown in Table 4, Table 5, and Table 6.

[0044] Table 4 Determination results of static saturated adsorption capacity of five resins

[0045] Resin type

polarity

Hawthorn total flavonoid adsorption (mg)

D-101

AB-8

SP825

HP20

D4020

non-polar

weak polarity

non-polar

non-polar

non-polar

11.37

11.09

11.42

7.48

5.87

[0046] Table 5 Desorption measu...

Embodiment 3

[0077] Embodiment 3 Pilot scale scale-up experiment

[0078] Weigh 15 kg of hawthorn decoction pieces, reflux extraction with 70% ethanol for 3 times, use 120 liters of ethanol for the first time, reflux extraction for 2 hours, use 90 liters of ethanol for the second and third times, reflux extraction for 1 hour respectively, and combine the extracts for 3 times , recover the ethanol until it has no alcohol smell, let it stand overnight, filter the precipitate with a filter cloth the next day, dilute to a solution containing 0.1 g of crude drug per ml, and set aside.

[0079] Soak 20 kg of pharmaceutical grade D101 macroporous resin with an appropriate amount of ethanol, put it on the column by wet method, and treat it for later use.

[0080] The extracted medicinal solution was loaded into the resin column twice, 75 liters each time, the flow rate of the sample was 2 times the column volume / hour, and the pH value was the pH value of the original medicinal solution (about pH 3...

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Abstract

Disclosed is an extraction and purification process of hawthorn flavonoid ingredients. The process is practiced in steps that firstly, hawthorn decoction pieces are dried and processed into particles with 3-8 mm diameter; the particles with ethanol with 70 percent of concentration are refluxed and extracted for three times; for the first time the particles and the ethanol with eight times of weight of the particles are extracted for two hours, and for the second and the third times, the particles and the ethanol with 6 times of weight of the particles are extracted for one hour; the liquid extractive is combined and decompressed for ethanol recovering, and then are condensed to extractive concentrated solution; secondly, water is added into the extractive concentrated solution until every milliliter of the extractive concentrated solution contains 0.1g of crude drug, the pH is regulated between 3 and 4, and then filtrate is produced after the solution is filtered; thirdly, the filtrate is made to pass through a D-101 macroporous resin column for adsorption, water washing and ethanol elution; lastly, the ethanol eluant is collected and condensed to the eluant with 1.1g per milliliter in consistency, and then the hawthorn extractive is produced after the condensed eluant is dried by spray. With the hawthorn extraction method, the total flavone transfer rate of hawthorn can be achieved to 79.5 per cent, and the total flavone content in the hawthorn extractive is calculated by rutin to be 24.6 per cent.

Description

technical field [0001] The invention relates to an extraction method of traditional Chinese medicine, in particular to an extraction method of hawthorn and its extract. Background technique [0002] Hawthorn is the dried and mature fruit of Crataegus pinnatifida Bge.var major.N.E.Br. or C. pinnatifida Bge. of the genus Hawthorn in the family Rosaceae, which was recorded in the 2005 edition of "Chinese Pharmacopoeia". It has the effects of eliminating food accumulation, promoting blood circulation and removing blood stasis. More than 150 kinds of components have been found and isolated from hawthorn (pulp, core and leaves), the main components are flavonoids, organic acids and so on. Flavonoids are the main active ingredients of hawthorn, and hyperoside, rutin, quercetin, and vitexin have been isolated. In recent years, raw hawthorn has been used in the clinical treatment of diseases such as hypertension, coronary heart disease and hyperlipidemia. Modern pharmacological st...

Claims

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Application Information

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IPC IPC(8): A61K36/34A61P3/06A61P9/10A61P9/12A61K131/00
Inventor 王光忠刘焱文陈树和何再安闫磊
Owner 湖北中医学院
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