Method for extracting and refining hydroxysafflor yellow A from safflower

A technology of hydroxy safflower and yellow pigment, which is applied in chemical instruments and methods, preparation of carbocyclic sugars, sugar derivatives, etc., can solve the problems of long cycle, unsolved, high price, etc.

Active Publication Date: 2012-09-19
HEBEI YILING MEDICINE INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN1475272A discloses a method for extracting and refining hydroxysafflower yellow A, which has the following disadvantages: 1. The process is "extraction-separation-alcohol precipitation-purification-re- Purification (1-3 times)", the whole process requires 5-7 steps, many process steps, long cycle, cumbersome, difficult to carry out practical operation in industrial production
2. It can be seen from experiments that the hydroxyl safflower yellow A in safflower has poor adsorption in weak polarity and medium polarity macroporous adsorption resins, and water can be eluted, and in strong polarity macroporous adsorption resins, the adsorption is extremely strong, and water and 95% ethanol cannot be eluted. In the separation, purification and repurification process of this patent, deionized water is used to elute impurities and hydroxysafflower yellow A. There is no method for monitoring the process, only to collect orange The fraction of the yellow color band is used as an indicator of the control process. Most of the components in safflower are orange-yellow, so the method of judging the elution end point by color has large errors, and the controllability of the separation, purification, and repurification processes is poor. Industrial production Difficult to operate
3. This patent uses polyamide or silica gel or dextran gel in the purification and repurification process. These three kinds of fillers are relatively expensive, especially dextran gel is expensive and difficult to regenerate. Methanol, For organic reagents such as ethanol and reagents such as acids and alkalis, the regeneration times and service life are not as good as those of macroporous adsorption resins. It must be filtered well, preferably through a 0.45um membrane, otherwise it is easy to block the chromatography column. In the pure precipitation process, a high concentration (60-90%) of ethanol or methanol or acetone is used. These organic reagents are harmful to the environment and human health. There is great harm, resulting in high cost and difficulty in industrial production
[0004] CN101195647A A also discloses a method for extracting and refining hydroxysafflower yellow A, which has the following disadvantages: 1. The process is "extraction-separation-purification-repurification (3 times)", the whole process requires 6 steps, many process steps, long cycle, cumbersome, difficult to carry out actual operation in industrial production
2. In the process of separation, purification, and repurification, deionized water is used to elute both impurities and hydroxysafflower yellow A. Although the Molisch and ninhydrin reactions are used to judge the end point of impurity removal in the separation process, the production Difficult to control, incomplete removal of impurities, easy loss of hydroxy safflower yellow A, purification and repurification process only collects orange-yellow ribbon fractions as an indicator of control process, most of the components in safflower are orange-yellow, use The method of judging the elution end point by color has a large error, so there is no effective monitoring method fo

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] a. Extraction: Weigh the safflower Chinese herbal medicine, add water to decoct 3 times, add water 23 times the weight of the Chinese herbal medicine added each time, except for the first soaking at room temperature for 30 minutes, then slightly boil for 20 minutes, and the rest are slightly boiled for 20 minutes. minutes, filter, combine the extracts, concentrate under reduced pressure below 60°C until the concentration of the crude drug is 0.25g / ml, and obtain the extract A;

[0056] b. The first purification: put the extract A and the weakly basic ion exchange resin D900 into the column according to the mass ratio - crude drug: resin ratio of 1:4, load the sample, saturate for 1 hour, and wash with deionized water of 15 times the column volume To neutrality, wash with 10% acetic acid at a concentration of 6 times column volume, and wash with 20 times column volume concentration of 4% ammonium acetate per hour at a flow rate of 8 times column volume per hour. The flow...

Embodiment 2

[0062] a. Extraction: Weigh the safflower Chinese herbal medicine, add water to decoct twice, add water 15 times the weight of the Chinese herbal medicine added each time, soak at room temperature for 20 minutes for the first time, boil for 10 minutes, and boil for 10 minutes for the second time. minutes, filter, combine the extracts, concentrate under reduced pressure below 60°C until the concentration of the crude drug is 0.25g / ml, and obtain the extract A;

[0063] b. The first purification: put the extract A and the weakly basic ion exchange resin D900 into the column according to the mass ratio-crude drug:resin ratio of 1:6, the diameter-to-height ratio of the chromatography is 1:6, and the sample loading flow rate is 2 times the column volume per hour, saturated for 2 hours, washed with 20 times the column volume of deionized water until neutral, 10 times the column volume concentration is 10% acetic acid washing, the flow rate is 10 times the column volume per hour, 20 t...

Embodiment 3

[0069] a. Extraction: Weigh the safflower Chinese herbal medicine, add water to decoct 3 times, add water 30 times the weight of the Chinese herbal medicine thrown in each time, except for the first soaking at room temperature for 60 minutes, then boil slightly for 40 minutes, and the remaining two times are slightly boiled. Boil for 40 minutes, filter, combine the extracts, concentrate under reduced pressure below 60°C until the concentration of the crude drug is 0.25g / ml, and obtain the extract A;

[0070] b. The first purification: put the extract A and the weakly basic ion exchange resin D900 into the column according to the mass ratio-crude drug:resin ratio of 1:2, the diameter-to-height ratio of the chromatography is 1:6, and the sample loading flow rate is 2 times the column volume per hour, saturated for 0.5 hours, washed with 10 times the column volume of deionized water to neutrality, washed with 10% acetic acid at a concentration of 5 times the column volume, the flo...

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PUM

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Abstract

The invention discloses a method for extracting and refining hydroxysafflor yellow A from safflower. The hydroxysafflor yellow A is a compound with a chalcone monoside structure, and is abundant in traditional Chinese medicinal material safflower (CARTHAMI FLOS). The hydroxysafflor yellow A with content of over 80 percent is obtained through the following five steps of: extracting form the traditional Chinese medicine safflower; purifying through ion exchange resin; purifying through neutral polarity macro-porous adsorption resin; purifying through non-polar macro-porous adsorption resin; and freeze-drying, wherein the transfer rate is over 20 percent.

Description

technical field [0001] The invention relates to a method for extracting and refining hydroxysafflower yellow A from safflower. Background technique [0002] Hydroxysafflor yellow A (hydroxysafflor yellow A) is a compound with a single chalcone glycoside structure, which is the most effective water-soluble part of safflower pharmacological effects, can inhibit platelet aggregation and release induced by platelet activating factor, and can compete with It can effectively inhibit the combination of platelet activating factor and platelet receptor, and is the active ingredient of safflower yellow for promoting blood circulation and removing blood stasis. It is a good raw material for medicine, it can also be used to make health care and cosmetics, and it is also a good food dye. Antiplatelet and anti-ischemic effects. Antithrombin-induced platelet aggregation activity, anti-inflammatory activity, cytoprotective activity, antitumor activity. [0003] CN1475272A discloses a met...

Claims

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Application Information

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IPC IPC(8): C07H7/04C07H1/08
Inventor 姜新刚赵韶华贾继明
Owner HEBEI YILING MEDICINE INST
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