Method for extracting and refining hydroxysafflor yellow A from safflower

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...

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 for the entire separation and purification process in the purification process, resulting in poor controllability of the process and difficult operation in industrial production

3. This patent uses dextran gel G-25 in the purification and repurification process. This filler is expensive, has limited regeneration times and service life, poor physical properties, small particles, and compact columns after packing, which is harmful to equipment, Samples and operators have high requirements, especially for purified samples, 0.45um membrane must be filtered, otherwise it is easy to block the chromatography column and cause the loss of Sephadex G-25, resulting in high cost and difficulty in industrial production, which is not easy to practice Applied to industrial production

[0005] CN101168539A also discloses a method for extracting hydroxysafflower yellow A, which is relatively simple and has the following disadvantages: this patent is only used for injection of Danhong Therefore, only the preliminary separation of hydroxysafflower yellow A in safflower was carried out, and the total content of salvianolic acid B and hydroxysafflower yellow A in the product Danhong for injection was more than 60%. The content of salvianolic acid B is more than 80%, and the mixing ratio of the two is that the weight ratio of salvia miltiorrhiza and safflower medicinal materials is 3:1. It can be seen that this patent is only a preliminary separation of hydroxyl safflower yellow A in safflower. Its purity is low, less than 20%

Although the safflower extract enhances the adsorption performance of the macroporous adsorption resin after acid adjustment, and then eluted with acid water, the hydroxy safflower yellow A is not eluted by acid water, and can be fully separated from impurities such as polysaccharides. The process is simple and convenient for industrial production, but its purity is low and cannot be used for the preparation of high-purity hydroxysafflower yellow A

[0006] CN101215307A discloses the extraction method of hydroxysafflower yellow A, and there are disadvantages as follows: 1. When the separation process does not solve the problem of water elution and impurity removal, the hydroxysafflower yellow The problem that impurities such as pigment A and polysaccharides are eluted together, the process can be poorly emptied, and it is not easy for industrial production

2. Although the whole process is simple, the exquisite process uses reversed-phase packing, which has high requirements for equipment, samples and personnel, especially for equipment, which should at least be able to pressurize elution and control the flow rate well. Conventional chromatography columns If the requirements cannot be met, the sample should be filtered with a 0.45um membrane to avoid clogging the chromatography column, which is not easy for actual industrial production

3. The price of the reversed-phase packing is more expensive than that of the macroporous adsorption resin in terms of regeneration times and limited service life. The eluent uses 10-70% ethanol, which has hidden dangers to the environment and personal safety.