A traditional Chinese medicine composition for treating gastric ulcer and its preparation process

Abstract

The present application relates to the technical field of traditional Chinese medicine, and specifically discloses a traditional Chinese medicine composition for treating gastric ulcers and its preparation process. The raw materials of the traditional Chinese medicine composition are composed of Asplenia and Cynanchum gracile; the preparation process of the traditional Chinese medicine composition comprises the following steps: crushing Asplenia and Cynanchum gracile, extracting with ethanol aqueous solution to obtain an extract, concentrating the extract to obtain an extractum, dissolving and dispersing the extractum with ethanol aqueous solution, adding grafted modified activated carbon for adsorption and impurity removal, solid-liquid separation, washing the grafted modified activated carbon with ethanol, combining the liquid phase, and concentrating to obtain the traditional Chinese medicine composition. The preparation process of the present application has the advantages of fully removing impurities and reducing the loss rate of effective ingredients. Since the present application fully removes ineffective ingredients such as protein and pectin, the loss rate of the effective ingredient acetophenone is reduced, and the dosage of the preparation is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicines, and in particular to a traditional Chinese medicine composition for treating gastric ulcer and a preparation process thereof. Background Art

[0002] Geshanxiao (Gypsophila) has the benefits of digestion, stomach strengthening, qi regulation, and pain relief; Styplenia has the benefits of clearing heat and detoxifying, and antibacterial and anti-inflammatory properties. The combination of the two can treat gastric and duodenal ulcers. Most of the substances in these Chinese medicinal herbs are soluble in water or ethanol and are generally extracted using water or ethanol. In addition to containing various active ingredients, the extracts also contain a large number of components that make up the various tissues and cell walls of the medicinal herbs, as well as the nutrients they store, such as starch, pectin, tannic acid, and protein. These have large molecular weights and exist as colloids in water. With a few exceptions, they generally have no pharmacological activity and are therefore generally referred to as impurities or ineffective substances. The presence of these many ineffective ingredients will not only affect the extraction efficiency of the target ingredients of traditional Chinese medicine, but also increase the dosage of the preparation, and even affect the appearance, stability and even efficacy of the medicine solution. For example, protein can easily cause the medicine solution to corrupt or precipitate, affecting the efficacy; taking drugs containing tannins can damage the intestinal mucosa, causing patients to have symptoms such as loss of appetite, nausea, and headaches; in summary, the presence of these impurities is the main factor that causes the current traditional Chinese medicine preparations to have a large dosage, poor stability, poor quality control system, and difficulty in conducting various high-efficiency, fast-acting, and long-acting new dosage forms.

[0003] The traditional method for separating and purifying traditional Chinese medicines (TCMs) in related technologies is water extraction and alcohol precipitation, which utilizes the different solubility of different substances in the extract in ethanol for separation and purification. This process is simple to operate, with relatively low technical and equipment costs, and can remove most impurities from TCM extracts. Therefore, this technique has certain advantages and is still used today.

[0004] Regarding the above-mentioned related technologies, although the water extraction and alcohol precipitation method can remove some impurities, it has the disadvantage of causing a large loss of effective ingredients. Summary of the Invention

[0005] In order to fully remove impurities and reduce the loss rate of effective ingredients, the present application provides a traditional Chinese medicine composition for treating gastric ulcer and a preparation process thereof.

[0006] In a first aspect, the present application provides a preparation process of a traditional Chinese medicine composition for treating gastric ulcer, which adopts the following technical solution:

[0007] A preparation process of a traditional Chinese medicine composition for treating gastric ulcer, wherein the raw materials of the traditional Chinese medicine composition are composed of Asplenia and Cyperus rotundus; the preparation process of the traditional Chinese medicine composition comprises the following steps:

[0008] The extract is concentrated to obtain an extract, the extract is dissolved and dispersed in an ethanol aqueous solution, and then a grafted modified activated carbon is added to perform adsorption and impurity removal, solid-liquid separation is performed, the grafted modified activated carbon is rinsed with ethanol, and the liquid phase is combined and concentrated to obtain a traditional Chinese medicine composition;

[0009] The preparation method of the grafted modified activated carbon comprises the following steps:

[0010] Surface modification: mixing activated carbon, sodium hydroxide solution and epichlorohydrin uniformly, heating for reaction, cooling, solid-liquid separation, washing to neutrality, and drying to obtain modified activated carbon;

[0011] Modification: uniformly mix the modified activated carbon, activated green 19 and water, adjust the pH to alkaline, heat to react, separate the solid and liquid, wash until colorless, then wash with methanol, and dry to obtain the modified activated carbon;

[0012] Graft modification: dissolve arginine in water, add N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and then add modified activated carbon to carry out grafting reaction. After the reaction is completed, wash, separate the solid and liquid, and dry to obtain grafted modified activated carbon.

[0013] By adopting the above technical scheme, since ethanol is a good solvent, the traditional alcohol precipitation process will remove some effective ingredients soluble in ethanol while removing impurities, such as acetophenone (2,5-dihydroxyacetophenone, 4-hydroxyacetophenone, Cynanchum multiflorum dibenzophenone and 2,4-dihydroxyacetophenone), and acetophenone is one of the main ingredients in Glechoma longituba used to treat gastric ulcers; the grafted modified activated carbon of the present application can fully adsorb and remove impurities such as protein and pectin, will not adsorb effective ingredients, and can be recycled; the present application adopts epichlorohydrin to react with the hydroxyl groups on the surface of activated carbon, grafts epichlorohydrin on the surface of activated carbon, and then uses active green 19 to react with epichlorohydrin to increase adsorption sites, and then grafts arginine onto active green 19. The carboxyl group of arginine reacts with the amino group of active green 19 to increase adsorption sites and reduce the adsorption steric hindrance, thereby increasing the adsorption performance of impurities such as protein and pectin, and will not adsorb effective ingredients.

[0014] Grafted modified activated carbon can adsorb pectin because there are amino groups on Reactive Green 19 and arginine. The positively charged amino groups produce electrical neutralization with the negatively charged pectin, resulting in an adsorption reaction; grafted modified activated carbon can adsorb protein because the multiple sulfonic acid groups in Reactive Green 19 can undergo electrostatic adsorption with proteins, the polyaromatic ring structure in Reactive Green 19 can undergo hydrophobic interaction with proteins for adsorption, and the amino groups on arginine can form hydrogen bonds with proteins to produce adsorption.

[0015] Optionally, the weight proportion of the Aspleniaceae is 245-420 parts, and the weight proportion of the Cyperus rotundus is 245-420 parts.

[0016] Optionally, the amount of grafted modified activated carbon added during the adsorption and impurity removal is 0.8-1 g / L.

[0017] By adopting the above technical solution, if the amount of grafted modified activated carbon added is too small, the impurity removal effect is poor; if the amount of grafted modified activated carbon added is too large, the production cost will be increased, and the impurity removal effect will not be significantly improved. Therefore, the amount of grafted modified activated carbon added during adsorption and impurity removal is preferably 0.8-1g / L.

[0018] Optionally, the temperature is controlled at 30-40°C during the adsorption removal.

[0019] By adopting the above technical solution, when the temperature is too low, the thermal motion of protein and pectin molecules is reduced and the adsorption effect is weakened; when the temperature is too high, the protein is easily inactivated and the glycosidic bonds on the pectin molecular chain are hydrolyzed, which is not conducive to adsorption. Therefore, the temperature is preferably controlled at 30-40°C during adsorption and impurity removal.

[0020] Optionally, the mass ratio of the modified activated carbon to activated green 19 is 1:(0.1-0.15).

[0021] By adopting the above technical solution and under the above ratio, sufficient active green 19 can be grafted onto the modified activated carbon.

[0022] Optionally, the mass ratio of the arginine to the modified activated carbon is 1:(1-2).

[0023] By adopting the above technical solution and under the above ratio, sufficient arginine can be grafted onto the modified activated carbon.

[0024] Optionally, the molar ratio of arginine, N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride is 3:(1-1.5):(1.5-2.5).

[0025] By adopting the above technical solution, the three raw materials are in the above ratio, which is conducive to the full reaction between the carboxyl group on arginine and the amino group on Reactive Green 19.

[0026] Optionally, the grafting reaction time is 8-12 hours.

[0027] By adopting the above technical solution, sufficient reaction time is conducive to the full reaction between the carboxyl group on arginine and the amino group on Reactive Green 19.

[0028] In a second aspect, the present application provides a traditional Chinese medicine composition for treating gastric ulcer, which is prepared by the above-mentioned preparation process.

[0029] In a third aspect, the present application provides a preparation for treating gastric ulcer, which adopts the following technical solution:

[0030] A preparation for treating gastric ulcer is prepared by adopting the above-mentioned traditional Chinese medicine composition. The preparation is in the form of granules, powders, tablets, pills or capsules.

[0031] By adopting the above technical solution, the present invention fully removes ineffective ingredients such as protein and pectin, thereby reducing the loss rate of the effective ingredient acetophenone and reducing the dosage of the preparation.

[0032] In summary, this application has the following beneficial effects:

[0033] 1. Since the present application uses epichlorohydrin to react with the hydroxyl groups on the surface of activated carbon, epichlorohydrin is grafted on the surface of the activated carbon, and then Reactive Green 19 is reacted with epichlorohydrin to increase the adsorption sites. Arginine is then grafted onto Reactive Green 19. The carboxyl group of arginine reacts with the amino group of Reactive Green 19 to increase the adsorption sites and reduce the adsorption steric hindrance, thereby increasing the adsorption performance of impurities such as protein and pectin without adsorbing the effective ingredients.

[0034] 2. Since the present application fully removes ineffective ingredients such as protein and pectin, the loss rate of the active ingredient acetophenone is reduced, and the dosage of the preparation is reduced. DETAILED DESCRIPTION

[0035] The present application is further described in detail below with reference to the embodiments.

[0036] Preparation example of grafted modified activated carbon

[0037] Preparation Example 1

[0038] The preparation method of the grafted modified activated carbon comprises the following steps:

[0039] Surface modification: 1 kg of activated carbon, 8 L of 1 mol / L sodium hydroxide aqueous solution and 3 L of epichlorohydrin were mixed evenly, the mesh size of the activated carbon was 100 mesh, heated to 40 ° C in a water bath, stirred for 10 hours, cooled to room temperature, filtered, washed with distilled water until the filtrate was neutral, and dried at 70 ° C to constant weight to obtain modified activated carbon;

[0040] Modification: 1 kg of modified activated carbon, 0.1 kg of active green 19 and 15 L of water were mixed evenly, sodium carbonate was added to adjust the pH to 10, heated to 80 ° C and stirred for 20 h, filtered, washed with distilled water until the filtrate was colorless, and then washed three times with a 10% volume fraction of methanol aqueous solution, and dried at 60 ° C to constant weight to obtain modified activated carbon;

[0041] Graft modification: 1 kg of arginine was dissolved in 10 L of water, and N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added. The molar ratio of arginine, N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride was 3:1:1.5. Then 0.5 kg of modified activated carbon was added for grafting reaction. The reaction time was 8 h. After the reaction was completed, it was washed with distilled water 3 times, filtered, and freeze-dried to obtain grafted modified activated carbon.

[0042] Preparation Example 2

[0043] The preparation method of the grafted modified activated carbon comprises the following steps:

[0044] Surface modification: 1 kg of activated carbon, 8 L of 1 mol / L sodium hydroxide aqueous solution and 3 L of epichlorohydrin were mixed evenly, the mesh size of the activated carbon was 100 mesh, heated to 40 ° C in a water bath, stirred for 10 hours, cooled to room temperature, filtered, washed with distilled water until the filtrate was neutral, and dried at 70 ° C to constant weight to obtain modified activated carbon;

[0045] Modification: 1 kg of modified activated carbon, 0.12 kg of active green 19 and 18 L of water were mixed evenly, sodium carbonate was added to adjust the pH to 10, heated to 80 ° C and stirred for 22 h, filtered, washed with distilled water until the filtrate was colorless, and then washed three times with a 10% volume fraction of methanol aqueous solution, and dried at 60 ° C to constant weight to obtain modified activated carbon;

[0046] Graft modification: 1 kg of arginine was dissolved in 10 L of water, and N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added. The molar ratio of arginine, N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride was 3:1.2:2. Then 0.5 kg of modified activated carbon was added for grafting reaction. The reaction time was 10 h. After the reaction was completed, it was washed with distilled water 3 times, filtered, and freeze-dried to obtain grafted modified activated carbon.

[0047] Preparation Example 3

[0048] The preparation method of the grafted modified activated carbon comprises the following steps:

[0049] Surface modification: 1 kg of activated carbon, 8 L of 1 mol / L sodium hydroxide aqueous solution and 3 L of epichlorohydrin were mixed evenly, the mesh size of the activated carbon was 100 mesh, heated to 40 ° C in a water bath, stirred for 10 hours, cooled to room temperature, filtered, washed with distilled water until the filtrate was neutral, and dried at 70 ° C to constant weight to obtain modified activated carbon;

[0050] Modification: 1 kg of modified activated carbon, 0.15 kg of active green 19 and 22.5 L of water were mixed evenly, sodium carbonate was added to adjust the pH to 10, heated to 80 ° C and stirred for 24 h, filtered, washed with distilled water until the filtrate was colorless, and then washed three times with a 10% volume fraction of methanol aqueous solution, and dried at 60 ° C to constant weight to obtain modified activated carbon;

[0051] Graft modification: 1 kg of arginine was dissolved in 10 L of water, and N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added. The molar ratio of arginine, N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride was 3:1.5:2.5. Then 0.5 kg of modified activated carbon was added for grafting reaction. The reaction time was 8 h. After the reaction was completed, the mixture was washed with distilled water 3 times, filtered, and freeze-dried to obtain grafted modified activated carbon.

[0052] Preparation Example 4

[0053] The difference from Preparation Example 2 is that the amount of modified activated carbon used is 1 kg.

[0054] Preparation Example 5

[0055] The difference from Preparation Example 2 is that the amount of modified activated carbon used is 1.5 kg.

[0056] Preparation Example 6

[0057] The difference from Preparation Example 2 is that the amount of modified activated carbon used is 2 kg.

[0058] Preparation Example 7

[0059] The difference from Preparation Example 2 is that the amount of modified activated carbon used is 2.5 kg.

[0060] Comparative Preparation Example 1

[0061] The preparation method of the grafted modified activated carbon comprises the following steps:

[0062] For surface modification, 1 kg of activated carbon, 8 L of 1 mol / L sodium hydroxide aqueous solution and 3 L of epichlorohydrin were mixed evenly, the mesh size of the activated carbon was 100 mesh, heated to 40 ° C in a water bath, stirred for 10 hours, cooled to room temperature, filtered, washed with distilled water until the filtrate was neutral, and dried at 70 ° C to constant weight to obtain grafted modified activated carbon.

[0063] Comparative Preparation Example 2

[0064] The preparation method of the grafted modified activated carbon comprises the following steps:

[0065] Surface modification: 1 kg of activated carbon, 8 L of 1 mol / L sodium hydroxide aqueous solution and 3 L of epichlorohydrin were mixed evenly, the mesh size of the activated carbon was 100 mesh, heated to 40 ° C in a water bath, stirred for 10 hours, cooled to room temperature, filtered, washed with distilled water until the filtrate was neutral, and dried at 70 ° C to constant weight to obtain modified activated carbon;

[0066] Load modification: chitosan was dissolved in acetic acid solution with a volume fraction of 0.5% to obtain a chitosan solution with a mass fraction of 0.5%. 1 kg of modified activated carbon was evenly mixed with the chitosan solution. The mass ratio of modified activated carbon to chitosan was 50:1. The mixture was allowed to stand, cooled, filtered, washed with distilled water until neutral, and dried at 80°C to obtain grafted modified activated carbon.

[0067] Comparative Preparation Example 3

[0068] The preparation method of the grafted modified activated carbon comprises the following steps:

[0069] Surface modification: 1 kg of activated carbon, 8 L of 1 mol / L sodium hydroxide aqueous solution and 3 L of epichlorohydrin were mixed evenly, the mesh size of the activated carbon was 100 mesh, heated to 40 ° C in a water bath, stirred for 10 hours, cooled to room temperature, filtered, washed with distilled water until the filtrate was neutral, and dried at 70 ° C to constant weight to obtain modified activated carbon;

[0070] Load modification: chitosan was dissolved in 0.5% by volume acetic acid solution to obtain a chitosan solution with a mass fraction of 0.5%, wherein the viscosity-average molecular weight of chitosan was 510,000 and the degree of deacetylation was 90%. 1 kg of modified activated carbon was mixed evenly with the chitosan solution at a mass ratio of modified activated carbon to chitosan of 50:1. The mixture was allowed to stand, cooled, filtered, washed with distilled water until neutral, and dried at 80°C to obtain loaded modified activated carbon.

[0071] Graft modification: 1 kg of arginine was dissolved in 10 L of water, and N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added. The molar ratio of arginine, N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride was 3:1.2:2. Then 0.5 kg of loaded modified activated carbon was added for grafting reaction. The reaction time was 10 h. After the reaction was completed, the mixture was washed with distilled water 3 times, filtered, and freeze-dried to obtain grafted modified activated carbon.

[0072] Example

[0073] Example 1

[0074] A traditional Chinese medicine composition for treating gastric ulcer, wherein the raw materials are composed of Asplenia gracilis and Cyperus rotundus in a mass ratio of 1:1;

[0075] The preparation process of the Chinese medicine composition comprises the following steps:

[0076] 245g of Asplenium truncatum and 245g of Cynanchum strychnifolium were crushed and extracted three times with 12 times the amount of 70% ethanol aqueous solution, each extraction time for 1.5h, filtered, the filtrates were combined, and the ethanol was recovered under reduced pressure to obtain an extract. The extract was concentrated to obtain an extract, which was dissolved and dispersed with 70% ethanol aqueous solution, and then grafted modified activated carbon was added for adsorption and impurity removal. The temperature was controlled at 30°C and the adsorption and impurity removal time was 12h. The grafted modified activated carbon was prepared by Preparation Example 1, and the amount of grafted modified activated carbon added was 0.8g / L. Filtered, the grafted modified activated carbon was rinsed with ethanol and the liquid phases were combined, the ethanol was recovered under reduced pressure, and concentrated to a relative density of 1.20 at room temperature to obtain a traditional Chinese medicine composition.

[0077] Examples 2-7

[0078] A traditional Chinese medicine composition for treating gastric ulcer is different from Example 1 in that the grafted modified activated carbon is prepared in sequence according to Preparation Examples 2-7.

[0079] Example 8

[0080] A traditional Chinese medicine composition for treating gastric ulcer, which is different from Preparation Example 5 in that the added amount of grafted modified activated carbon is 0.9 g / L.

[0081] Example 9

[0082] A traditional Chinese medicine composition for treating gastric ulcer, which is different from Preparation Example 5 in that the added amount of grafted modified activated carbon is 1 g / L.

[0083] Example 10

[0084] A traditional Chinese medicine composition for treating gastric ulcer, which is different from Preparation Example 8 in that the temperature is controlled at 35°C during adsorption and impurity removal.

[0085] Example 11

[0086] A traditional Chinese medicine composition for treating gastric ulcer, which is different from Preparation Example 8 in that the temperature is controlled at 40°C during adsorption and impurity removal.

[0087] Comparative Example

[0088] Comparative Examples 1-3

[0089] A traditional Chinese medicine composition for treating gastric ulcer is different from Example 2 in that the grafted modified activated carbon is prepared in sequence from Comparative Preparation Examples 1-3.

[0090] Comparative Example 4

[0091] A traditional Chinese medicine composition for treating gastric ulcer, which differs from Example 2 in that the grafted modified activated carbon is replaced by ordinary activated carbon of the same weight.

[0092] Comparative Example 5

[0093] A traditional Chinese medicine composition for treating gastric ulcer, the preparation process of which comprises the following steps:

[0094] Crush 420g of Aspleniaceae and 420g of Cynanchum wilfordii, add 12 times the amount of water and boil three times, the first time for 2 hours, the second time for 1.5 hours, and the third time for 1 hour. Combine the decoctions, filter, and concentrate the filtrate to an extract with a relative density of 1.20 (80°C). When the extract is cooled to 40°C, add 2 times the amount of ethanol, mix well, let it stand for 24 hours, take the supernatant, filter, recover the ethanol, and concentrate to an extract with a relative density of 1.25 (80°C) to obtain a traditional Chinese medicine composition.

[0095] Application Example 1

[0096] A granule for treating gastric ulcer is prepared from 500 g of a traditional Chinese medicine composition and 9500 g of sucrose. The traditional Chinese medicine composition is prepared according to Example 2. The preparation method of the granule comprises the following steps: uniformly mixing the traditional Chinese medicine composition and sucrose, granulating, and drying to obtain the granule.

[0097] Usage and dosage: Take with boiled water, 15g at a time, 2 to 3 times a day.

[0098] Application Example 2

[0099] A tablet for treating gastric ulcer, comprising 8450 g of a traditional Chinese medicine composition, 1000 g of starch, 500 g of talc, and 50 g of magnesium stearate, wherein the traditional Chinese medicine composition is prepared according to Example 2;

[0100] The preparation method of the tablet comprises the following steps: uniformly mixing the traditional Chinese medicine composition, starch, talcum powder and magnesium stearate, screening the particles with a 14-mesh sieve, and tableting to obtain tablets.

[0101] Usage and dosage: Oral, 3 tablets at a time, 3 times a day.

[0102] Specifications: 0.3g per tablet.

[0103] Application Example 3

[0104] A capsule for treating gastric ulcer, prepared from 9000 g of a traditional Chinese medicine composition and 1000 g of starch, wherein the traditional Chinese medicine composition is prepared according to Example 2;

[0105] The preparation method of the capsule comprises the following steps: uniformly mixing the traditional Chinese medicine composition and starch, drying, and filling the mixture into capsules.

[0106] Usage and Dosage: Oral, 3 tablets at a time, 3 times a day.

[0107] Specifications: 0.3g per capsule.

[0108] Performance testing

[0109] Detection method

[0110] (1) Acetophenone content test: 2.0 g of each of the extract and the Chinese medicine composition in Examples 1-11 and Comparative Examples 1-5 were accurately weighed and placed in a flat-bottom flask. 25 nL of methanol was accurately added and weighed. The mixture was heated under reflux for 2 h. The mixture was cooled and weighed. The amount lost was supplemented with methanol. The mixture was mixed and filtered. The filtrate was centrifuged at 10,000 rpm for 10 min. The supernatant was collected to obtain the test solution for later use. A Synergi 4μ Hydro-RP 80A column (4.6 mm × 250 mm, 4 μm) was used. The mobile phase was methanol (A)-0.1% phosphoric acid aqueous solution (B). The gradient elution was performed (0-24 min, 15% A→21% A; 24-35 min, 21% A; 35-36 min, 21% A→23% A; 36-60 min, 23% A). The flow rate was 1.0 mL min. -1 , detection wavelengths were 260 nm (3-hydroxy-4-methoxybenzoic acid, 2,5-dihydroxyacetophenone) and 280 nm (4-hydroxyacetophenone, Cynanchum multiflorum benzophenone, 2,4-dihydroxyacetophenone), column temperature was 35°C, injection volume was 10 μL, the content of acetophenone (2,5-dihydroxyacetophenone, 4-hydroxyacetophenone, Cynanchum multiflorum benzophenone and 2,4-dihydroxyacetophenone) in the extract was m0, the content of acetophenone in the traditional Chinese medicine composition was m1, and the acetophenone loss rate = (m0-m1) / m0*100%.

[0111] (2) Pectin removal rate test: 2.0 g of each of the extracts and the Chinese medicine composition in Examples 1-11 and Comparative Examples 1-5 were accurately weighed, and the pectin content in the extracts and the Chinese medicine composition was tested by the carbazole-sulfuric acid colorimetric method. The pectin content in the extracts was M0, and the pectin content in the Chinese medicine composition was M1. The pectin removal rate = (M0-M1) / M0*100%.

[0112] (3) Protein Removal Rate Test: 2.0 g of each of the extracts and the Chinese medicinal compositions from Examples 1-11 and Comparative Examples 1-5 were accurately weighed and the protein content of the extracts and the Chinese medicinal compositions was determined using Coomassie Brilliant Blue staining. The protein content in the extracts was designated as D0, and the protein content in the Chinese medicinal compositions was designated as D1. Protein removal rate = (D0 - D1) / D0 * 100%. The test results are shown in Table 1.

[0113] Table 1 Test results

[0114]

[0115]

[0116] Combining Examples 1-3 and Comparative Examples 1-5 with Table 1, it can be seen that Comparative Example 5 uses an alcohol precipitation method to remove impurities such as pectin and protein, with a low removal rate and a high loss rate of the effective substance acetophenone. Comparative Example 4 uses ordinary activated carbon for adsorption and impurity removal, and the acetophenone loss rate is higher than that of Comparative Example 5, while the pectin removal rate and protein removal rate are lower than those of Comparative Example 5, indicating that the adsorption and impurity removal effect of ordinary activated carbon is poor. After the activated carbon is surface modified in Comparative Example 1, the acetophenone loss rate is lower than that of Comparative Example 4, while the pectin removal rate and protein removal rate are higher than those of Comparative Example 4, indicating that epichlorohydrin reacts with the hydroxyl groups on the surface of the activated carbon. The adsorption sites were increased, the pectin removal rate and protein removal rate were improved, and the acetophenone loss rate was reduced; Examples 1-3 were grafted with Reactive Green 19 and arginine on the basis of Comparative Example 1, which greatly improved the pectin removal rate and protein removal rate, and greatly reduced the acetophenone loss rate. This may be because the grafting of epichlorohydrin, Reactive Green 19 and arginine increased the adsorption sites and reduced the adsorption steric hindrance. Among them, the effect of Example 2 was better; Comparative Example 2 was loaded with chitosan on the basis of Comparative Example 1, and the acetophenone loss rate was lower than that of Comparative Example 1, and the pectin removal rate and protein removal rate were higher than those of Comparative Example 1, indicating that chitosan also has the effect of improving The results show that the pectin removal rate, protein removal rate and acetophenone loss rate can be reduced by 10%. In Comparative Example 3, based on Example 2, Reactive Green 19 is replaced by arginine. The acetophenone loss rate is lower than that of Comparative Example 2 but much higher than that of Example 2. The pectin removal rate and protein removal rate are higher than those of Comparative Example 2 but much lower than that of Example 2. This may be because after chitosan is loaded on the surface of activated carbon, some adsorption sites are combined with activated carbon, resulting in a decrease in adsorption capacity. In Examples 4-7, the amount of modified activated carbon is increased in sequence. The acetophenone loss first decreases and then increases, and the pectin removal rate and protein removal first increase and then decrease. Among them, the effect of Example 5 is better, indicating that the chitosan is more effective. The mass ratio of amino acid to modified activated carbon has a great influence on the adsorption and impurity removal performance; Examples 8-9 increase the amount of grafted modified activated carbon in turn, the acetophenone loss rate gradually decreases, and the pectin removal rate and protein removal rate gradually increase, but the improvement effect of Example 9 is not obvious. Taking all factors into consideration, the effect of Example 8 is better; Examples 10-11 increase the adsorption temperature in turn, the acetophenone loss first decreases and then increases, and the pectin removal rate and protein removal first increase and then decrease. This is because at low temperature, the thermal motion of protein and pectin molecules decreases, and the adsorption effect weakens; high temperature easily inactivates protein and hydrolyzes the glycosidic bonds on the pectin molecular chain, which is not conducive to adsorption.

[0117] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A preparation process of a Chinese medicine composition for treating gastric ulcer, characterized in that: The raw materials of the traditional Chinese medicine composition are composed of Asplenia and Cyperus rotundus; The preparation process of the Chinese medicine composition comprises the following steps: The extract is concentrated to obtain an extract, the extract is dissolved and dispersed in an ethanol aqueous solution, and then a grafted modified activated carbon is added to perform adsorption and impurity removal, solid-liquid separation is performed, the grafted modified activated carbon is rinsed with ethanol, and the liquid phase is combined and concentrated to obtain a traditional Chinese medicine composition; The preparation method of the grafted modified activated carbon comprises the following steps: Surface modification: mixing activated carbon, sodium hydroxide solution and epichlorohydrin uniformly, heating for reaction, cooling, solid-liquid separation, washing to neutrality, and drying to obtain modified activated carbon; Modification: uniformly mix the modified activated carbon, activated green 19 and water, adjust the pH to alkaline, heat to react, separate the solid and liquid, wash until colorless, then wash with methanol, and dry to obtain the modified activated carbon; Graft modification: dissolve arginine in water, add N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and then add modified activated carbon to carry out grafting reaction. After the reaction is completed, wash, separate the solid and liquid, and dry to obtain grafted modified activated carbon.

2. The preparation process of a Chinese medicine composition for treating gastric ulcer according to claim 1, characterized in that: The amount of grafted modified activated carbon added during the adsorption and impurity removal is 0.8-1 g / L.

3. The preparation process of a Chinese medicine composition for treating gastric ulcer according to claim 1, characterized in that: The temperature is controlled at 30-40°C during the adsorption and impurity removal.

4. The preparation process of a Chinese medicine composition for treating gastric ulcer according to claim 1, characterized in that: The mass ratio of the modified activated carbon to activated green 19 is 1:(0.1-0.15).

5. The preparation process of a Chinese medicine composition for treating gastric ulcer according to claim 1, characterized in that: The mass ratio of the arginine to the modified activated carbon is 1:(1-2).

6. The preparation process of a Chinese medicine composition for treating gastric ulcer according to claim 1, characterized in that: The molar ratio of arginine, N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride is 3:(1-1.5):(1.5-2.5).

7. The preparation process of a Chinese medicine composition for treating gastric ulcer according to claim 1, characterized in that: The grafting reaction time is 8-12 hours.

8. A Chinese medicine composition for treating gastric ulcer, characterized in that: The invention is prepared by the preparation process according to any one of claims 1 to 7.

9. A preparation for treating gastric ulcer, characterized in that: The preparation is prepared using the traditional Chinese medicine composition according to claim 8, wherein the preparation is in the form of granules, powders, tablets, pills or capsules.

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