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Chrysanthemum total flavone resin purification method

A purification method and a technology of total flavonoids, applied in organic chemistry and other fields, can solve problems such as low yield, troublesome elution, and unsatisfactory, and achieve the effects of good reproducibility, large adsorption capacity, and easy operation

Inactive Publication Date: 2003-12-10
浙江现代中药与天然药物研究院有限公司 +1
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Problems solved by technology

[0003] Traditionally, solvent extraction and polyamide column chromatography are used for the purification of traditional Chinese medicine flavonoids. However, the solvent extraction method is cumbersome to operate, and the extraction process is easy to emulsify. The organic solvents used, such as chloroform, ethyl acetate, and n-butanol, have different levels. In addition, if the total flavonoids of chrysanthemum are extracted with chloroform, only 4% of the total amount of flavonoids can be obtained; with ethyl acetate extraction, only 50% of the total amount can be obtained; with n-butanol extraction, only 40% of the total amount can be obtained. %, so it is necessary to use the above solvents to extract in order to make the total flavonoids basically completely extracted
The polyamide purification method has an irreversible adsorption of 40% of the total flavonoids of chrysanthemum, so the yield is low and the elution is troublesome
Therefore above-mentioned two kinds of methods are all unsatisfactory in the purification of chrysanthemum total flavonoids

Method used

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  • Chrysanthemum total flavone resin purification method
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  • Chrysanthemum total flavone resin purification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1 A kind of purification method of the present invention

[0021] (1) Extraction of chrysanthemum: chrysanthemum was extracted three times by reflux with 70% ethanol, the three filtrates were combined, concentrated under reduced pressure to a certain volume, filtered, and set aside.

[0022] (2) Resin pretreatment: Soak the macroporous resin in 95% ethanol for 24 hours, pack the column, wash the column with 95% ethanol until the effluent is diluted 5 times with water and is not turbid, rinse the chromatography column with deionized water until the effluent No ethanol smell.

[0023] (3) Putting on the column: put the chrysanthemum extract on the column, control the flow rate of the effluent to 1BV / h, until the extract completely enters the resin bed, and let it stand still for 0.5-1 hour to allow it to fully absorb.

[0024] (4) Elution: Rinse the resin bed with 2BV of deionized water, control the flow rate of the effluent to 1BV / h, to remove the part that i...

Embodiment 2

[0025] Example 2 Select different conditions for purification

[0026] Adopt the method provided by the present invention, select different conditions to carry out chrysanthemum total flavonoid purification experiment, the results are shown in Table 1: the experimental results under different conditions in Table 1

[0027] Experiment Total flavonoid transfer rate Total flavonoid content

[0028] Elution flow rate Loading ratio Ethanol concentration Elution volume

[0029] Numbering (%) (%)

[0030] 1 2Bv / h 1:2 50% 2Bv 77.7 70.6

[0031] 2 2Bv / h 1:3 70% 2.5Bv 98.9 68.0

[0032] 3 2Bv / h 1:5 90% 3Bv 100.0 70.0

[0033] 4 3Bv / h 1:2 70% 3Bv 93.8 61.5

[0034] 5 3Bv / h 1:3 90% 2Bv 97.3 65.0

[0035] 6 3Bv / h 1:5 50% 2.5Bv 100.6 72.4

[0036] 7 4Bv / h 1:2 90% 2.5Bv 92.2 63.7

[0037] 8 4Bv / h 1:3 50% 3Bv 91.3 71.8

[0038] 9 4Bv / h 1:5 70% 2Bv 100.9 68.0

[0039] 10 2Bv / h 1:4 70% 2Bv 96.5 67.6

[0040] 11 2B...

Embodiment 3

[0042] Example 3 Under optimized conditions, tests were carried out on four different chromatographic columns, and the results are shown in Table 2:

[0043] Table 2 Comparison of results of macroporous resin purification of total flavonoids from chrysanthemum on chromatographic columns of different specifications

[0044] Column specifications Loading amount (g) Flavonoid transfer rate (%) Total flavonoid content of purified product (%)

[0045]2.5cm×30cm 13 99.3±3.6 65.6±0.4

[0046] 3.5cm×60cm 130 100.2±2.2 66.9±1.7

[0047] 10cm×100cm 2000 99.7±3.8 67.5±2.9

[0048] 20cm×160cm 15000 95.6±4.2 67.3±2.5

[0049] n=3

[0050] It can be seen from Table 2 that the total flavonoids of chrysanthemums are purified by macroporous resin, the transfer rate of total flavonoids is high, and the content of total flavonoids in the purified product reaches more than 65%. Moreover, the macroporous resin purification method has good reproducibility on chromatographic columns of differen...

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Abstract

The present invention adopts macroporous resin adsorption to make chrysanthemum extract undergo the processes of resin column treatment, elution, collecting elute, concentrating and drying so as to obtain the purified chrysanthemum total flavone. The transferrin rate of its total flavone can be up to above 95%, and its purified total flavone content can be up to above 65%, its reproducibility is good, and said resin can be repeatedly used.

Description

technical field [0001] The invention belongs to a method for purifying traditional Chinese medicine components, and mainly relates to a method for purifying Chinese medicine extracts, in particular to a method for purifying total flavonoids from chrysanthemums. Background technique [0002] Chrysanthemum contains flavonoids, volatile oils, polysaccharides and other ingredients. It is traditionally used to evacuate wind-heat, clear liver and improve eyesight. Modern research shows that chrysanthemum has anti-cardiovascular disease, lowering blood fat, anti-fatigue, anti-oxidation and other effects. Many studies believe that these effects of chrysanthemum are closely related to its flavonoids. Due to the complex composition of the total extract of chrysanthemum, the preparations made inevitably have the disadvantages of being thick, large, and black, and the total extract also has relatively high hygroscopicity because it contains more sugars, which limits its dosage form. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30
Inventor 蒋惠娣胡季强陈忆庭曾苏
Owner 浙江现代中药与天然药物研究院有限公司
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