CN111454253A - Method for purifying and decoloring traditional Chinese medicine monomer vitexin - Google Patents

Abstract

The invention discloses a method for purifying and decoloring vitexin as a traditional Chinese medicine monomer, which adopts an activated carbon decoloring combined film filtration method and finally adopts ethanol crystallization to obtain a high-purity vitexin raw material with good color and luster. The active carbon is added in the production process of the traditional Chinese medicine injection, which is beneficial to adsorbing pigment and removing pyrogen; after decarburization, macromolecular pigments are effectively intercepted by adopting microfiltration without introducing new substances; finally, the high-purity vitexin is obtained by low-temperature refrigeration and crystallization. The process has low production cost and convenient operation, and does not introduce new harmful substances.

Description

Method for purifying and decoloring traditional Chinese medicine monomer vitexin

Technical Field

The invention relates to a method for processing a traditional Chinese medicine monomer plant medicine, in particular to a method for purifying and decoloring the plant medicine, and more particularly to a method for purifying and decoloring a traditional Chinese medicine monomer vitexin.

Background

Vitexin is a single compound extracted from leaves of Crataegus pinnatifida of Rosaceae, and has purity of more than 98%. The patent application with publication No. CN103509002A discloses a method for extracting vitexin, and a powder injection prepared by adding appropriate adjuvants is clinically applied. The product is not marketed and sold at home and abroad, and belongs to a new medicine of Chinese medicine. The pharmacological action of the compound shows that the compound has the effects of resisting experimental myocardial ischemia, protecting rat myocardial ischemia reperfusion injury, protecting isolated rat myocardial ischemia reperfusion injury and the like. The vitexin is clinically suitable for treating cardiovascular diseases such as coronary heart disease, myocardial infarction, angina pectoris and the like. The traditional Chinese medicine injection is the highest-level embodiment of traditional Chinese medicine modernization, the research, registration and approval threshold of the traditional Chinese medicine injection is gradually improved, and the obsolescence of the injection varieties which are backward, have unclear components and have unclear mechanisms is in great tendency. Therefore, the quality control of vitexin has to be high standard and strict requirement, and safety guarantee is provided for clinical use.

The clinical dosage form of vitexin is injection, and has specific strict standard requirements on color, purity and the like; and the product is obtained by extracting, separating and purifying traditional Chinese medicine hawthorn leaves, so that the purification and decoloration steps are extremely important in the production process of the vitexin raw material.

The existing method for extracting and purifying the traditional Chinese medicine monomer basically comprises a resin adsorption method, an activated carbon adsorption method, a precipitation method, a filtration method and the like, and the pigment is difficult to be completely removed when the decoloration processes are independently applied; therefore, the method considers the combined application and combines the clinical application formulation of the vitexin to be injection, and various new substances are avoided to be introduced as much as possible in the production process, thereby establishing the specific purification and decoloration process of the vitexin.

Disclosure of Invention

The invention provides a method for purifying and decoloring vitexin as a traditional Chinese medicine monomer aiming at the problems of decoloring and purifying traditional Chinese medicine monomer products. The method adopts an activated carbon decoloration combined film filtration method and finally adopts ethanol crystallization, so that the vitexin raw material with high purity and good color can be obtained. The active carbon is added in the production process of the traditional Chinese medicine injection, which is beneficial to adsorbing pigment and removing pyrogen; after decarburization, macromolecular pigments are effectively intercepted by adopting microfiltration without introducing new substances; finally, the high-purity vitexin is obtained by low-temperature refrigeration and crystallization. The process has low production cost and convenient operation, and does not introduce new harmful substances.

The purification and decoloration method of the traditional Chinese medicine monomer vitexin comprises the following steps:

step 1: preparing 1-5% vitexin ethanol solution through the vitexin crude product; the preparation method of the crude vitexin used in the invention is shown in CN 103509002A.

Step 2: adding active carbon for injection into the vitexin ethanol solution obtained in the step 1, and stirring for 0.5 hour at 60 ℃;

and step 3: decarburizing and filtering the mixed solution obtained in the step 2, and filtering the mixed solution through a 0.45um microporous filter membrane;

and 4, step 4: and (4) refrigerating and crystallizing the vitexin ethanol solution filtered in the step (3) at a low temperature to obtain a vitexin decolored and purified product.

In step 1, the solvent used for preparing the ethanol solution of vitexin is 60 vt% ethanol.

In the step 2, the adding proportion of the needle-use activated carbon is 1.0-3.0 g/L.

In the step 3, the decarburizing and filtering method is titanium rod filter filtering.

And 4, controlling the temperature of low-temperature refrigeration crystallization to be 2-8 ℃.

The method removes alcohol-insoluble impurities by dissolving vitexin with an ethanol solution; adopting activated carbon to adsorb and decolor to remove pigment impurities, and matching with a membrane filtration operation to remove macromolecular impurities; finally, removing alcohol-soluble impurities by low-temperature crystallization of ethanol liquid; the method realizes separation of various pigments and impurities from the vitexin product, achieves the aim of color removal and purification, obtains the high-purity vitexin product, and provides a safety guarantee basis for the preparation of the vitexin product.

Drawings

FIG. 1 is an HP L C chromatogram of crude vitexin.

FIG. 2 is a HP L C chromatogram of a pure vitexin obtained by the present invention.

Detailed Description

Example 1:

the method for purifying and decoloring vitexin in the embodiment comprises the following steps of:

1. taking 10g crude vitexin (purity of 84.7%), adding 1L 60% ethanol solution, heating and stirring for dissolving to obtain vitexin ethanol solution;

2. adding activated carbon for injection into the ethanol solution obtained in the step 1, wherein the concentration of the activated carbon is 1.0 g/L;

3. keeping the temperature of the ethanol solution in the step 2 at 60 ℃, and stirring for 0.5 hour;

4. the mixed solution in the step 3 is decarburized and filtered, and is filtered through a 0.45um microporous filter membrane;

5. refrigerating the filtered vitexin ethanol solution at the low temperature of 2 ℃ for crystallization to obtain 7.6g of yellow vitexin powder with the purity of 99.1%.

Example 2:

the method for purifying and decoloring vitexin in the embodiment comprises the following steps of:

1. taking 25g of crude vitexin (with purity of 84.7%), adding 1L 60% ethanol solution, heating and stirring for dissolving to obtain vitexin ethanol solution;

2. adding activated carbon for injection into the ethanol solution obtained in the step 1, wherein the concentration of the activated carbon is 2.0 g/L;

3. keeping the temperature of the ethanol solution in the step 2 at 60 ℃, and stirring for 0.5 hour;

4. the mixed solution in the step 3 is decarburized and filtered, and is filtered through a 0.45um microporous filter membrane;

5. refrigerating the filtered vitexin ethanol solution at the low temperature of 5 ℃ for crystallization to obtain 18.9g of yellow vitexin powder with the purity of 99.3%.

Example 3:

the method for purifying and decoloring vitexin in the embodiment comprises the following steps of:

1. taking 50g of crude vitexin (purity of 84.7%), adding 1L 60% ethanol solution, heating and stirring for dissolving to obtain vitexin ethanol solution;

2. adding activated carbon for injection into the ethanol solution obtained in the step 1, wherein the concentration of the activated carbon is 3.0 g/L;

3. keeping the temperature of the ethanol solution in the step 2 at 60 ℃, and stirring for 0.5 hour;

4. the mixed solution in the step 3 is decarburized and filtered, and is filtered through a 0.45um microporous filter membrane;

5. refrigerating the filtered vitexin ethanol solution at the low temperature of 8 ℃ for crystallization to obtain 37.4g of yellow vitexin powder with the purity of 99.6%.

Example 4:

the selection of the solvent in the method for purifying and decolorizing vitexin in this example is based on:

taking five crude vitexin products (1.0 g of each part), respectively adding 1L parts of acetone, absolute ethyl alcohol, 90% ethyl alcohol, 60% ethyl alcohol and 30% ethyl alcohol, heating to dissolve, adding 2.0 g/L parts of active carbon, stirring for 0.5 hour at 60 ℃, decarburizing, filtering by using a microporous membrane, refrigerating and crystallizing at the low temperature of 5 ℃, and inspecting the purification and crystallization conditions of the product in different media, thereby determining the solvents used for crystallization, wherein the test results are shown in table 1.

TABLE 1 results of crystallization selection test with different solvents

The test result shows that 60% ethanol is used as the crystallization solvent, and the yield, the appearance color and the purity of the crystallization solvent are better controlled, so 60% ethanol is selected as the crystallization solvent.

Example 5:

in this embodiment, the usage amount of activated carbon in the purifying and decolorizing method of vitexin is selected according to:

1. activated carbon usage test

Two parts of vitexin 60% ethanol solution 1L are taken, 2.0g of activated carbon is added respectively, the mixture is stirred for 30 minutes under different temperature conditions (25 ℃, 60 ℃ and 90 ℃), decarburized and filtered, and the color change conditions before and after the solution is compared by observation (the effect before and after the solution is decolorized is evaluated by the solution light transmittance), and the results are shown in Table 2.

TABLE 2 results of activated carbon usage test

Test results show that the vitexin ethanol solution is added with 2.0 g/L of activated carbon, and the decoloring effect is better after stirring for 30 minutes at the constant temperature of 60 ℃ in a water bath.

2. Test for amount of active carbon

Taking 5 parts of vitexin 60% ethanol solution, adding 0.5g, 1.0g, 2.0g, 3.0g and 4.0g of activated carbon for injection into each part of 1L, stirring for 30 minutes at constant temperature of 60 ℃ in water bath, decarburizing and filtering, observing the color change before and after decoloring of the comparative solution (the decoloring effect is evaluated by the solution light transmittance), and comparing the loss change after the adsorbed vitexin component is adsorbed, wherein the results are shown in Table 3.

TABLE 3 test results of the amount of activated carbon used

The test result shows that when the vitexin ethanol solution is added with the activated carbon with different concentrations, the decolorization effect is increased along with the increase of the consumption of the activated carbon after stirring for 30 minutes at the constant temperature of 60 ℃ in a water bath, but the loss rate of the vitexin content is increased along with the increase of the consumption of the activated carbon.

Example 6:

in the purification and decolorization method of vitexin in this example, the crystallization conditions are selected according to the following:

taking two parts (1.0 g of each part) of crude vitexin, respectively adding 1L of 60% ethanol, heating to dissolve, adding 2.0 g/L of active carbon, stirring at 60 ℃ for 0.5 hour, decarburizing, filtering with a microporous membrane, refrigerating at room temperature of 25-30 ℃ and low temperature of 2-8 ℃ for crystallization, observing crystallization conditions of the product under different temperature conditions, observing the color of separated vitexin, and determining the yield and content of vitexin, wherein the results are shown in Table 4.

Table 4 recrystallization conditions test results

Test results show that the vitexin crystallization yield is high when the vitexin is refrigerated at the low temperature of 2-8 ℃, and the content and related substances meet the requirements, so the vitexin is refrigerated at the low temperature of 2-8 ℃ for crystallization.

Example 7:

and (3) purifying and decoloring vitexin:

1. adding 60% ethanol solution into reaction kettle, heating to 60 deg.C, adding crude vitexin, stirring to dissolve vitexin completely, wherein the solution color is brown red, the crude vitexin is brown powder, and HP L C content is 85.6%, as shown in figure 1.

2. Adding active carbon into the vitexin ethanol solution, adsorbing and decolorizing with needle, decarbonizing, filtering with membrane, refrigerating at low temperature, separating out crystal, filtering, and collecting yellow solid filter cake to obtain pure vitexin product, which is yellow powder with HP L C content of 99.6% and total impurities of 0.37%, as shown in figure 2.

The method has the advantages of low cost of obtaining products, completely qualified color, high content, simple operation and suitability for production.

The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and the technical scheme also comprises the technical scheme formed by any combination of the technical characteristics.

While the foregoing is directed to embodiments of the present invention, it will be appreciated by those skilled in the art that various changes may be made in the embodiments without departing from the principles of the invention, and that such changes and modifications are intended to be included within the scope of the invention.

Claims (6)

1. A method for purifying and decoloring traditional Chinese medicine monomer vitexin is characterized by comprising the following steps:

and (3) decoloring by adopting activated carbon and combining with a membrane filtration method, and finally crystallizing by adopting ethanol to obtain the high-purity vitexin raw material.

2. The purification and decolorization method according to claim 1, characterized by comprising the steps of:

step 1: preparing 1-5 wt% of an ethanol solution of vitexin by using the crude vitexin product;

step 2: adding active carbon for injection into the vitexin ethanol solution obtained in the step 1, and stirring for 0.5 hour at 60 ℃;

and step 3: decarburizing and filtering the mixed solution obtained in the step 2, and filtering the mixed solution through a 0.45um microporous filter membrane;

and 4, step 4: and (4) refrigerating and crystallizing the vitexin ethanol solution filtered in the step (3) at a low temperature to obtain a vitexin decolored and purified product.

3. The purification and decolorization method according to claim 2, characterized in that:

in step 1, the solvent used for preparing the ethanol solution of vitexin is 60 vt% ethanol.

4. The purification and decolorization method according to claim 2, characterized in that:

in the step 2, the adding proportion of the needle-use activated carbon is 1.0-3.0 g/L.

5. The purification and decolorization method according to claim 2, characterized in that:

in the step 3, the decarburizing and filtering method is titanium rod filter filtering.

6. The purification and decolorization method according to claim 2, characterized in that:

and 4, controlling the temperature of low-temperature refrigeration crystallization to be 2-8 ℃.

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