A gastrointestinal tract regulating product prepared by using marine green algae plants

Abstract

The present invention specifically relates to a gastrointestinal tract regulating product prepared by using marine green algae. Rhamnose, the main component of Enteromorpha polysaccharide, is a cyclic molecular structure. Rhamnose is alkalized into alkalinized rhamnose, and the alkalinized rhamnose is reacted with chloroacetic acid to obtain carboxymethyl rhamnolate. Carboxymethyl rhamnolate is acidified in an acid solution to form carboxymethyl rhamnoic acid. After adding aluminum hydroxide, carboxymethyl rhamnoic acid and aluminum ions react to form carboxymethyl rhamnoic acid aluminum with a cross-linked structure. The structure of carboxymethyl rhamnoic acid aluminum with a cross-linked structure is more stable, ensuring that aluminum ions play a role after entering the gastrointestinal tract, and aluminum ions are quickly released and protect the gastric mucosa in the case of excessive gastric acid. The Enteromorpha polysaccharide component in the gastrointestinal tract regulating product prepared by the present invention can increase gastrointestinal motility, and the combination of aluminum ions and Enteromorpha polysaccharide can better regulate the gastrointestinal tract.

Description

Technical Field

[0001] The present invention particularly relates to a product capable of regulating the gastrointestinal tract which is prepared by utilizing marine green algae plants. Background Art

[0002] Enteromorpha is a common marine green algae plant, widely distributed in the eastern coastal areas of my country, with the richest resources in the Qingdao waters. According to the Compendium of Materia Medica, Enteromorpha can be used as both medicine and food, and has extremely high nutritional value. Haida Biology and Ocean University of China extracted various effective ingredients such as polysaccharides, proteins, and minerals from Enteromorpha. Among them, the polysaccharides in Enteromorpha are the main active ingredients in Enteromorpha. They are sulfated polysaccharides, including rhamnose, xylose, glucose, etc., and have multiple functions such as anti-oxidation and hypolipidemic.

[0003] In the medical field, aluminum ions can neutralize gastric acid, reduce the stimulation of gastric acid on aluminum ions, and form a protective film on the surface of gastric mucosa, which plays a role in protecting gastric mucosa. Using enteromorpha to make aluminum-containing products is not only rich in raw materials, natural and non-toxic, but also has the effects of protecting gastric mucosa and promoting gastrointestinal motility. There is no product in the prior art that combines the two. Summary of the invention

[0004] In order to solve the problems existing in the prior art, the present invention provides a gastrointestinal tract regulating product prepared by using marine green algae plants, thereby achieving the invention purpose of simultaneously protecting the gastric mucosa and promoting gastrointestinal motility.

[0005] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0006] A gastrointestinal tract regulating product prepared by using marine green algae, the preparation method of the product comprising the following steps:

[0007] S1. Purification

[0008] The dried Enteromorpha is broken into 300-500 mesh, added into deionized water, heated to 100-120°C and extracted for 2-3 hours, filtered, the filtrate is concentrated under reduced pressure to an extract, and added into an ethanol solution to obtain a precipitate, the precipitate is separated and dissolved in deionized water, and Enteromorpha polysaccharide is obtained after dialysis and freeze-drying.

[0009] Preferably, the mass ratio of the dried enteromorpha to deionized water is 1:20-30.

[0010] Preferably, the mass of the extract is 50-60% of the mass of the filtrate.

[0011] Preferably, the mass ratio of the extract to the ethanol solution is 1:3-5; the mass fraction of the ethanol solution is 92-97%.

[0012] Preferably, the molecular weight of the dialysis is 3500Da; the temperature of the freeze-drying is -15 to -10°C, and the time is 12 to 18 hours.

[0013] The rhamnose content of the Enteromorpha polysaccharide is greater than 67%, and the xylose content is greater than 20%.

[0014] S2. Alkalization

[0015] The enteromorpha polysaccharide is dissolved in deionized water, and then an alkali solution is added to carry out an alkalization reaction to obtain an alkalized enteromorpha polysaccharide solution.

[0016] Preferably, the mass ratio of the enteromorpha polysaccharide to deionized water is 1:9-12.

[0017] Preferably, the alkaline solution is a potassium hydroxide solution or a sodium hydroxide solution, and the amount of the alkaline solution added is 11-14% of the mass of the Enteromorpha polysaccharide in the alkaline solution.

[0018] Preferably, the alkalization reaction is carried out at a temperature of 40 to 50° C. and for a time of 60 to 80 minutes.

[0019] S3, etherification

[0020] Chloroacetic acid is added to the alkaline Enteromorpha polysaccharide solution to carry out etherification reaction, and after the reaction is completed, it is precipitated with anhydrous ethanol and freeze-dried to obtain the etherified Enteromorpha polysaccharide.

[0021] Preferably, the amount of chloroacetic acid added is 17.5-21% of the mass of Enteromorpha polysaccharide.

[0022] Preferably, the temperature of the etherification reaction is 50-65° C. and the time is 50-70 min.

[0023] Preferably, the freeze-drying temperature is -15 to -10°C and the time is 12 to 18 hours.

[0024] S4, acidification

[0025] The etherified Enteromorpha polysaccharide is dissolved in an acid solution and acidified to obtain a carboxymethylated Enteromorpha polysaccharide solution.

[0026] Preferably, the acid solution is an aqueous solution of hydrochloric acid with a mass fraction of 1 to 3%.

[0027] Preferably, the acidification time is 4 to 6 hours.

[0028] S5, Composite

[0029] Aluminum agent is added to the carboxymethylated Enteromorpha polysaccharide solution and stirred evenly, the temperature is raised to 40-50° C. for reaction for 3-4 hours, and the product capable of regulating the gastrointestinal tract is obtained after filtering and freeze-drying.

[0030] Preferably, the aluminum agent is aluminum hydroxide.

[0031] Preferably, the added amount of the aluminum agent is 5-8% of the mass of the etherified Enteromorpha polysaccharide.

[0032] Rhamnose, the main component of Enteromorpha polysaccharide, is a cyclic molecular structure. The substituents on some carbon positions of rhamnose can undergo substitution reactions with sodium hydroxide or potassium hydroxide to alkalize rhamnose into alkaline rhamnose, which then reacts with chloroacetic acid to obtain carboxymethyl rhamnolate. Carboxymethyl rhamnolate is acidified in acid solution to remove potassium or sodium to form carboxymethyl rhamnoic acid. After adding aluminum hydroxide, the carboxymethyl Enteromorpha polysaccharide solution is acidic, and aluminum hydroxide releases aluminum ions in the solution. Since aluminum ions are positive trivalent, one aluminum ion can combine with three carboxylate ions, and the three carboxylate ions are connected to the same aluminum. Therefore, carboxymethyl rhamnoic acid reacts with aluminum ions to form carboxymethyl rhamnoic acid aluminum with a cross-linked structure. The cross-linked structure of carboxymethyl rhamnoic acid aluminum is more stable, ensuring that aluminum ions play a role after entering the gastrointestinal tract. In the case of excessive gastric acid, aluminum ions are quickly released and protect the gastric mucosa.

[0033] Due to the adoption of the above technical solution, the technical effects achieved by the present invention are:

[0034] 1. The gastrointestinal tract regulating product prepared by the present invention has abundant raw materials, high nutritional value, can be produced on a large scale, and has high economic benefits.

[0035] 2. The gastrointestinal tract regulating product prepared by the present invention can not only release aluminum ions to neutralize gastric acid and protect gastric mucosa after consumption, but also the polysaccharide components of Enteromorpha can increase gastrointestinal motility. The combination of aluminum ions and Enteromorpha polysaccharides can better regulate the gastrointestinal tract.

[0036] 3. In the gastrointestinal tract regulating product prepared by the present invention, since the aluminum carboxymethyl rhamnolate therein has a cross-linked structure, the aluminum ions are more stable and mild in effect, and are quickly released in the gastric acid environment, but will not excessively adjust the pH of the gastric environment, thereby ensuring that the aluminum ions play a role in neutralizing gastric acid and protecting the gastric mucosa after entering the gastrointestinal tract. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 is the reaction formula for the alkalization of rhamnose;

[0038] Figure 2 is the reaction formula for the etherification of alkalized rhamnose;

[0039] Figure 3 This is the reaction formula for the acidification of carboxymethyl rhamnoic acid;

[0040] Figure 4 Schematic diagram of the reaction of carboxymethyl rhamnoic acid and aluminum hydroxide. DETAILED DESCRIPTION

[0041] The present invention is further described below in conjunction with specific embodiments.

[0042] Example 1: A gastrointestinal tract regulating product prepared by using marine green algae, the preparation method of the product comprising the following steps:

[0043] S1. Purification

[0044] The dried Enteromorpha was broken into 400 mesh, added into deionized water, heated to 110°C and extracted for 3 hours. After filtering, the filtrate was concentrated under reduced pressure to obtain an extract, and added into an ethanol solution to obtain precipitate A. The precipitate A was separated and dissolved in deionized water, and then dialyzed and freeze-dried to obtain Enteromorpha polysaccharide.

[0045] The mass ratio of the dried enteromorpha to deionized water is 1:25.

[0046] The mass of the extract is 55% of the mass of the filtrate.

[0047] The mass ratio of the extract to the ethanol solution is 1:4; the mass fraction of the ethanol solution is 95%.

[0048] The molecular weight of the dialysis was 3500Da; the temperature of the freeze-drying was -12°C and the time was 16h.

[0049] The rhamnose in the Enteromorpha polysaccharide accounts for 70.3%, and the xylose accounts for 22.1%.

[0050] S2. Alkalization

[0051] The enteromorpha polysaccharide is dissolved in deionized water, and then a sodium hydroxide solution is added to carry out an alkalization reaction to obtain an alkalized enteromorpha polysaccharide solution.

[0052] The mass ratio of the Enteromorpha polysaccharide to deionized water is 1:10.

[0053] The amount of sodium hydroxide solution added is 13% of the mass of Enteromorpha polysaccharide in the sodium hydroxide solution.

[0054] The alkalization reaction was carried out at a temperature of 45° C. and for 70 minutes.

[0055] S3, etherification

[0056] Chloroacetic acid is added to the alkaline Enteromorpha polysaccharide solution to carry out etherification reaction, and after the reaction is completed, it is precipitated with anhydrous ethanol and freeze-dried to obtain the etherified Enteromorpha polysaccharide.

[0057] The amount of chloroacetic acid added is 19% of the mass of Enteromorpha polysaccharide.

[0058] The temperature of the etherification reaction is 60° C. and the time is 60 min.

[0059] The freeze-drying temperature is -12°C and the time is 16 hours.

[0060] S4, acidification

[0061] The etherified Enteromorpha polysaccharide is dissolved in an acid solution and acidified to obtain a carboxymethylated Enteromorpha polysaccharide solution.

[0062] The acid solution is an aqueous solution of hydrochloric acid with a mass fraction of 2%.

[0063] The acidification time is 5h.

[0064] S5, Composite

[0065] Aluminum agent was added to the carboxymethylated Enteromorpha polysaccharide solution and stirred evenly, the temperature was raised to 45°C for reaction for 3.5 hours, and the product capable of regulating the gastrointestinal tract was obtained after filtering and freeze-drying.

[0066] The aluminum agent is aluminum hydroxide.

[0067] The added amount of the aluminum agent is 7% of the mass of the etherified Enteromorpha polysaccharide.

[0068] Example 2: A gastrointestinal tract regulating product prepared by using marine green algae, the preparation method of the product comprising the following steps:

[0069] S1. Purification

[0070] The dried Enteromorpha was broken into 500 mesh, added into deionized water, heated to 100°C and extracted for 2 hours, filtered, the filtrate was concentrated under reduced pressure to obtain an extract, and added into an ethanol solution to obtain precipitate A, which was separated and dissolved in deionized water, dialyzed and freeze-dried to obtain Enteromorpha polysaccharide.

[0071] The mass ratio of the dried enteromorpha to deionized water is 1:20.

[0072] The mass of the extract is 50% of the mass of the filtrate.

[0073] The mass ratio of the extract to the ethanol solution is 1:3; the mass fraction of the ethanol solution is 92%.

[0074] The molecular weight of the dialysis was 3500Da; the temperature of the freeze-drying was -15°C and the time was 12h.

[0075] The rhamnose in the Enteromorpha polysaccharide accounts for 67.6%, and the xylose accounts for 21.5%.

[0076] S2. Alkalization

[0077] The enteromorpha polysaccharide is dissolved in deionized water, and then a sodium hydroxide solution is added to carry out an alkalization reaction to obtain an alkalized enteromorpha polysaccharide solution.

[0078] The mass ratio of the Enteromorpha polysaccharide to deionized water is 1:9.

[0079] The amount of sodium hydroxide solution added is such that the sodium hydroxide in the sodium hydroxide solution accounts for 11% of the mass of Enteromorpha polysaccharide.

[0080] The temperature of the alkalization reaction is 40° C. and the time is 60 min.

[0081] S3, etherification

[0082] Chloroacetic acid is added to the alkaline Enteromorpha polysaccharide solution to carry out etherification reaction, and after the reaction is completed, it is precipitated with anhydrous ethanol and freeze-dried to obtain the etherified Enteromorpha polysaccharide.

[0083] The amount of chloroacetic acid added is 17.5% of the mass of Enteromorpha polysaccharide.

[0084] The temperature of the etherification reaction is 50° C. and the time is 50 min.

[0085] The freeze-drying temperature is -15°C and the time is 12 hours.

[0086] S4, acidification

[0087] The etherified Enteromorpha polysaccharide is dissolved in an acid solution and acidified to obtain a carboxymethylated Enteromorpha polysaccharide solution.

[0088] The acid solution is an aqueous solution of hydrochloric acid with a mass fraction of 1%.

[0089] The acidification time is 6 hours.

[0090] S5, Composite

[0091] Aluminum agent was added to the carboxymethylated Enteromorpha polysaccharide solution and stirred evenly, the temperature was raised to 40°C for reaction for 3 hours, and the product capable of regulating the gastrointestinal tract was obtained after filtering and freeze-drying.

[0092] The aluminum agent is aluminum hydroxide.

[0093] The added amount of the aluminum agent is 5% of the mass of the etherified Enteromorpha polysaccharide.

[0094] Example 3: A gastrointestinal tract regulating product prepared by using marine green algae, the preparation method of the product comprising the following steps:

[0095] S1. Purification

[0096] The dried Enteromorpha was broken into 300 mesh, added into deionized water, heated to 120°C and extracted for 2 hours. After filtering, the filtrate was concentrated under reduced pressure to obtain an extract, and added into an ethanol solution to obtain precipitate A. The precipitate A was separated and dissolved in deionized water, and Enteromorpha polysaccharide was obtained after dialysis and freeze-drying.

[0097] The mass ratio of the dried enteromorpha to deionized water is 1:30.

[0098] The mass of the extract is 60% of the mass of the filtrate.

[0099] The mass ratio of the extract to the ethanol solution is 1:5; the mass fraction of the ethanol solution is 97%.

[0100] The molecular weight of the dialysis was 3500Da; the temperature of the freeze-drying was -10°C and the time was 18h.

[0101] The rhamnose in the Enteromorpha polysaccharide accounts for 69.3%, and the xylose accounts for 21.3%.

[0102] S2. Alkalization

[0103] The enteromorpha polysaccharide is dissolved in deionized water, and then a potassium hydroxide solution is added to carry out an alkalization reaction to obtain an alkalized enteromorpha polysaccharide solution.

[0104] The mass ratio of the Enteromorpha polysaccharide to deionized water is 1:12.

[0105] The amount of potassium hydroxide solution added is such that the potassium hydroxide in the potassium hydroxide solution accounts for 14% of the mass of Enteromorpha polysaccharide.

[0106] The temperature of the alkalization reaction is 50° C. and the time is 80 min.

[0107] S3, etherification

[0108] Chloroacetic acid is added to the alkaline Enteromorpha polysaccharide solution to carry out etherification reaction, and after the reaction is completed, it is precipitated with anhydrous ethanol and freeze-dried to obtain the etherified Enteromorpha polysaccharide.

[0109] The amount of chloroacetic acid added is 21% of the mass of Enteromorpha polysaccharide.

[0110] The temperature of the etherification reaction is 65° C. and the time is 70 min.

[0111] The freeze-drying temperature is -10°C and the time is 18 hours.

[0112] S4, acidification

[0113] The etherified Enteromorpha polysaccharide is dissolved in an acid solution and acidified to obtain a carboxymethylated Enteromorpha polysaccharide solution.

[0114] The acid solution is an aqueous solution of hydrochloric acid with a mass fraction of 3%.

[0115] The acidification time is 4h.

[0116] S5, Composite

[0117] Aluminum agent was added to the carboxymethylated Enteromorpha polysaccharide solution and stirred evenly, the temperature was raised to 50° C. for reaction for 4 hours, and the product capable of regulating the gastrointestinal tract was obtained after filtering and freeze-drying.

[0118] The aluminum agent is aluminum hydroxide.

[0119] The added amount of the aluminum agent is 8% of the mass of the etherified Enteromorpha polysaccharide.

[0120] 3 g of the gastrointestinal tract regulating product prepared in Examples 1-3 was added into 200 ml of artificial gastric juice with a pH of 0.8 to test its release effect and neutralization effect. See Table 1 for details.

[0121] Table 1

[0122]

[0123] As can be seen from Table 1, the gastrointestinal tract regulating products prepared in Examples 1-3 can quickly release and neutralize gastric acid in the case of excessive gastric acid secretion, with a fast neutralization rate, and a low maximum pH of gastric acid after neutralization, which avoids the stimulation of continued gastric acid secretion by too high pH of gastric acid after neutralization, and the effect is mild and non-irritating. At the same time, the polysaccharide component of Enteromorpha can increase gastrointestinal motility, and the combination of aluminum ions and Enteromorpha polysaccharides can better regulate the gastrointestinal tract.

[0124] Unless otherwise specified, the ratios and percentages described in the present invention are all weight ratios and weight percentages; and the raw materials are all commercially available.

[0125] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention is described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A gastrointestinal tract regulating product prepared by using marine green algae, characterized in that: The preparation method of the product includes purification, alkalization, etherification, acidification and compounding; The purification comprises the following steps: breaking the dried Enteromorpha into 300-500 meshes, adding the mixture into deionized water, heating the mixture to 100-120° C. and extracting the mixture for 2-3 hours, filtering the mixture, concentrating the filtrate under reduced pressure into an extract, and adding the extract into an ethanol solution to obtain a precipitate, separating the precipitate and dissolving it in deionized water, and obtaining Enteromorpha polysaccharide after dialysis and freeze-drying. The alkalization step is to dissolve the Enteromorpha polysaccharide in deionized water, and then add an alkaline solution to carry out an alkalization reaction to obtain an alkaline Enteromorpha polysaccharide solution; The etherification comprises adding chloroacetic acid to the alkaline Enteromorpha polysaccharide solution to carry out an etherification reaction, and after the reaction is completed, precipitating with anhydrous ethanol and freeze-drying to obtain the etherified Enteromorpha polysaccharide; The acidification is to dissolve the etherified Enteromorpha polysaccharide in an acid solution and acidify it to obtain a carboxymethylated Enteromorpha polysaccharide solution; The compounding comprises adding an aluminum agent to a carboxymethylated enteromorpha polysaccharide solution and stirring evenly, heating to 40-50° C. to react for 3-4 hours, filtering, freeze-drying, and obtaining a product capable of regulating the gastrointestinal tract; The aluminum agent is aluminum hydroxide; The amount of the aluminum agent added is 5-8% of the mass of the etherified Enteromorpha polysaccharide.

2. The gastrointestinal tract regulating product prepared by using marine green algae according to claim 1, characterized in that: The mass ratio of the dried Enteromorpha to deionized water is 1:20-30; the mass of the extract is 50-60% of the mass of the filtrate; the mass ratio of the extract to the ethanol solution is 1:3-5; the mass fraction of the ethanol solution is 92-97%; the freeze-drying temperature is -15--10°C, and the time is 12-18h; the proportion of rhamnose in the Enteromorpha polysaccharide is greater than 67%, and the proportion of xylose is greater than 20%.

3. The gastrointestinal tract regulating product prepared by using marine green algae according to claim 1, characterized in that: The mass ratio of the Enteromorpha polysaccharide to deionized water is 1:9-12; the alkaline solution is a potassium hydroxide solution or a sodium hydroxide solution, and the amount of the alkaline solution added is that the potassium hydroxide or sodium hydroxide in the alkaline solution accounts for 11-14% of the mass of the Enteromorpha polysaccharide; the temperature of the alkalization reaction is 40-50°C, and the time is 60-80 minutes.

4. The gastrointestinal tract regulating product prepared by using marine green algae according to claim 1, characterized in that: The amount of chloroacetic acid added is 17.5-21% of the mass of Enteromorpha polysaccharide; the temperature of the etherification reaction is 50-65°C, and the time is 50-70 minutes; the temperature of the freeze-drying is -15--10°C, and the time is 12-18 hours.

5. The gastrointestinal tract regulating product prepared by using marine green algae according to claim 1, characterized in that: The acid solution is an aqueous solution of hydrochloric acid with a mass fraction of 1 to 3%; the acidification time is 4 to 6 hours.

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