CN115154407A - Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent - Google Patents

Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent Download PDF

Info

Publication number
CN115154407A
CN115154407A CN202210162581.3A CN202210162581A CN115154407A CN 115154407 A CN115154407 A CN 115154407A CN 202210162581 A CN202210162581 A CN 202210162581A CN 115154407 A CN115154407 A CN 115154407A
Authority
CN
China
Prior art keywords
chitosan
flaxseed gum
cross
linked hydrogel
hydrogel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202210162581.3A
Other languages
Chinese (zh)
Other versions
CN115154407B (en
Inventor
吴良平
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Hualiang Engine Network Technology Co ltd
Original Assignee
Youdao Tianjin Health Consulting Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Youdao Tianjin Health Consulting Co ltd filed Critical Youdao Tianjin Health Consulting Co ltd
Priority to CN202210162581.3A priority Critical patent/CN115154407B/en
Publication of CN115154407A publication Critical patent/CN115154407A/en
Application granted granted Critical
Publication of CN115154407B publication Critical patent/CN115154407B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/70Carbohydrates; Sugars; Derivatives thereof
    • A61K31/715Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
    • A61K31/716Glucans
    • A61K31/722Chitin, chitosan
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/55Linaceae (Flax family), e.g. Linum
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02Inorganic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0012Galenical forms characterised by the site of application
    • A61K9/0053Mouth and digestive tract, i.e. intraoral and peroral administration
    • A61K9/0065Forms with gastric retention, e.g. floating on gastric juice, adhering to gastric mucosa, expanding to prevent passage through the pylorus
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/06Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • A61P3/04Anorexiants; Antiobesity agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • A61P3/06Antihyperlipidemics

Abstract

The invention discloses chitosan flaxseed gum cross-linked hydrogel and a preparation method thereof, and application of the chitosan flaxseed gum cross-linked hydrogel in a gastric filler, and relates to the field of medical assistance. The chitosan flaxseed gum cross-linked hydrogel comprises the following components in parts by weight: and (3) chitosan: 100 parts of a binder; flaxseed gum: 10-30 parts; calcium salt: 0.1-1 part, wherein the average molecular weight of the chitosan is 30-100 kDa, and the deacetylation degree is 80-100 percent. The chitosan flaxseed gum cross-linked hydrogel prepared by the method adopts a physical cross-linking mode to form a hydrogel three-dimensional network structure, has higher pH sensitivity and high swelling ratio in gastric juice, does not have a chemical cross-linking reaction process in the synthesis process, and is safer and simpler in process control; meanwhile, the chitosan and the flaxseed gum also have the functions of losing weight and reducing fat, and can actively adjust the weight of a user.

Description

Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent
Technical Field
The invention relates to the field of medical assistance, in particular to chitosan flaxseed gum cross-linked hydrogel and a preparation method thereof, and application of the chitosan flaxseed gum cross-linked hydrogel in a gastric bulking agent.
Background
The hydrogel is a three-dimensional network polymer with stronger hydrophilicity, has good water absorption performance, can be quickly swelled to store a large amount of water without dissolving after contacting with water, and simultaneously keeps certain strength. The characteristics of the hydrogel make the hydrogel an ideal raw material of a gastric filler, can effectively occupy the stomach space and provide satiety, assists a user to control and regulate diet, and does not cause serious side effects on a human body, however, most of high-strength hydrogels are difficult to degrade in physiological microorganisms or respond to environmental stimuli, have insufficient pH sensitivity, and influence the swelling ratio of the hydrogel in gastric juice.
Meanwhile, the existing stomach filler does not have the physiological function of directly regulating the weight of a user, and the long-term process of taking the stomach filler to assist weight loss is inevitable, so that the stomach filler does not have competitive advantages in increasingly abundant weight loss treatment approaches.
Disclosure of Invention
The invention provides chitosan flaxseed gum cross-linked hydrogel, a preparation method and application thereof in gastric bulking agents, which can improve pH sensitivity and swelling ratio of the hydrogel and have the physiological function of directly regulating the weight of a user.
In order to solve the technical problems, the invention provides a chitosan flaxseed gum crosslinked hydrogel which comprises the following components in parts by weight: and (3) chitosan: 100 parts of (A); flaxseed gum: 10-30 parts; calcium salt: 0.1-1 part, wherein the average molecular weight of the chitosan is 30-100 kDa, and the deacetylation degree is 80-100 percent.
By adopting the scheme, when in use, the commonly used chitosan, flaxseed gum and calcium chloride in the additive are evaluated as raw materials, the raw materials are harmless to human bodies and have high safety, the chitosan with higher deacetylation degree and lower average molecular weight is selected to meet better solubility and dissolution efficiency, carboxyl contained in the flaxseed gum can mutually generate electrostatic interaction with ammonium ions generated when the chitosan is dissolved in an acidic solution, so that a physical crosslinking site is formed, meanwhile, galacturonic acid contained in the flaxseed gum is positioned in the main chain of molecules and can be contacted with calcium ions in the calcium chloride to generate bridging action, so that a hydrogel three-dimensional network is formed, and when the flaxseed gum is used as a gastric filler, the situation that the swelling ratio in acidic gastric juice is higher, the hydrogel can be dispersed after entering an alkaline colon environment, the pH sensitivity and the swelling ratio are high, and satiety is provided; meanwhile, the chitosan and the flaxseed gum have the functions of losing weight and reducing fat, and can actively regulate the weight of a user.
Preferably, the calcium salt is one or more of calcium chloride, calcium gluconate, calcium lactate and calcium hydrogen phosphate.
Preferably, the composition comprises the following components in parts by weight: and (3) chitosan: 100 parts of (A); flaxseed gum: 15-20 parts of a stabilizer; calcium salt: 0.3 to 0.6 portion.
As a preferred scheme, the calcium salt is calcium chloride, and the mass ratio of the linseed glue to the calcium chloride is 25:1.
In order to solve the above technical problems, the second object of the present invention is to provide a method for preparing a chitosan flaxseed gum crosslinked hydrogel, comprising the following steps:
(1) Mixing flaxseed gum with calcium salt under heat preservation, and dissolving in pure water to obtain a premixed solution; dissolving chitosan in an organic acid aqueous solution to prepare a chitosan solution;
(2) Mixing the premixed solution and the chitosan solution under the condition of heat preservation, uniformly stirring, and dropwise adding an alkali solution to adjust the pH value to obtain a mixture;
(3) And cooling the mixture, freezing, repeatedly freezing and thawing, cleaning and drying to obtain the hydrogel particles.
Preferably, in the step (1), the chitosan solution has a mass fraction of 5% -10%, and the organic acid aqueous solution is an acetic acid solution with a volume fraction of 0.5% -2%.
Preferably, in the step (1), the mass fraction of the flaxseed gum in the flaxseed gum solution is 5-10%.
Preferably, in step (2), the pH is adjusted to 4.5 to 6.5.
As a preferred scheme, in the step (1), the heat preservation temperature is 80-90 ℃, and the mixing and stirring time is 6-12h; in the step (3), the temperature of the freezing treatment is-60 ℃ to-20 ℃ for 6-125h, and the freezing and thawing are repeated for 1-3 times.
In order to solve the technical problems, the invention also provides an application of the chitosan flaxseed gum cross-linked hydrogel in a gastric bulking agent.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
1. the chitosan, the flaxseed gum and the calcium chloride used in the application belong to the types of common food additives, are harmless to human bodies, have high safety, do not produce secondary products, and are harmless to human organs.
2. The chitosan flaxseed gum cross-linked hydrogel prepared by the method adopts a physical cross-linking mode to form a hydrogel three-dimensional network structure, has higher pH sensitivity and high swelling ratio in gastric juice, does not have a chemical cross-linking reaction procedure in the synthesis process, and is safer and simpler in process control.
3. The chitosan flaxseed gum cross-linked hydrogel obtained in the application can fill stomach space to provide satiety, and the used raw material components, namely chitosan and flaxseed gum, have the functions of losing weight and reducing fat, and can actively adjust the weight of a user.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example one
A chitosan flaxseed gum cross-linked hydrogel can be applied to the field of gastric bulking agents, and comprises the following steps:
(1) According to the mass ratio of 10:1, weighing 10kg of flaxseed gum by mass and 1kg of calcium salt which can be calcium chloride, calcium gluconate, calcium lactate or calcium hydrophosphate and the like, wherein the calcium salt is specifically calcium chloride, continuously stirring for 12 hours at the temperature of 80 ℃, dissolving in purified water, and continuously keeping the temperature at 80 ℃ for standby to obtain a flaxseed gum solution with the mass fraction of 5%;
(2) Weighing 100kg of chitosan according to a proportion, wherein the average molecular weight of the chitosan is 100kDa, the deacetylation degree range is 95%, and dissolving the chitosan in an acetic acid solution with the mass fraction of 2% to prepare a chitosan solution with the mass fraction of 10%;
(3) Mixing the prepared linseed gum solution and the chitosan solution under the condition of 80 ℃ heat preservation, carrying out homogeneous stirring at the speed of 1000r/min for 30min, dropwise adding a sodium hydroxide solution with the concentration of 0.1mol/L in the process, and adjusting the pH value to 4.5 to obtain a mixture;
(4) Naturally cooling the mixture to room temperature, freezing for 6 hours at-60 ℃ in a low-temperature refrigerator, naturally thawing at room temperature, repeatedly freezing and thawing for 3 times, and repeatedly washing the frozen and thawed product with purified water for 4 times;
(5) Freeze-drying the freeze-thaw product at-80 deg.C/24 h, and grinding and sieving the product to obtain dried hydrogel particles with particle size not more than 2 mm.
Example two
A chitosan flaxseed gum cross-linked hydrogel can be applied to the field of gastric bulking agents, and comprises the following steps:
(1) According to the mass ratio of 25: weighing 15kg of flaxseed gum and 0.6kg of calcium chloride in a proportion of 1, continuously stirring for 12 hours at 85 ℃, dissolving in purified water, and continuously keeping the temperature at 85 ℃ for standby application to obtain a flaxseed gum solution with the mass fraction of 7%;
(2) Weighing 100kg of chitosan according to a proportion, wherein the average molecular weight of the chitosan is 80kDa, the deacetylation degree range is 90%, and dissolving the chitosan in an acetic acid solution with the mass fraction of 1% to prepare a chitosan solution with the mass fraction of 8%;
(3) Mixing the prepared linseed gum solution and chitosan solution under the condition of heat preservation at 85 ℃, uniformly stirring at 2000r/min for 15min, dropwise adding a sodium hydroxide solution with the concentration of 0.5mol/L in the process, and adjusting the pH value to 5 to obtain a mixture;
(4) Naturally cooling the mixture to room temperature, freezing the mixture in a low-temperature refrigerator for 8 hours at-40 ℃, naturally thawing the mixture at room temperature, repeatedly freezing and thawing for 3 times, and repeatedly washing the frozen and thawed products with purified water for 4 times;
(5) Freeze-drying the freeze-thaw product at the temperature of minus 80 ℃/24h, and grinding and screening the obtained product to obtain the dried hydrogel particles with the particle size not more than 2 mm.
EXAMPLE III
A chitosan flaxseed gum cross-linked hydrogel can be applied to the field of gastric bulking agents and comprises the following steps:
(1) According to the mass ratio of 200:3, weighing 20kg of flaxseed gum and 0.3kg of calcium chloride in a mass ratio, continuously stirring for 12 hours at 90 ℃, dissolving in purified water, and continuously keeping the temperature at 90 ℃ for standby to obtain a flaxseed gum solution with the mass fraction of 9%;
(2) Weighing 100kg of chitosan according to a proportion, wherein the average molecular weight of the chitosan is 50kDa, the deacetylation degree range is 85 percent, and dissolving the chitosan into an acetic acid solution with the mass fraction of 0.5 percent to prepare a chitosan solution with the mass fraction of 6 percent;
(3) Mixing the prepared flaxseed gum solution and chitosan solution under the condition of heat preservation at 90 ℃, uniformly stirring at 3000r/min for 10min, dropwise adding a sodium hydroxide solution with the concentration of 1mol/L in the process, and adjusting the pH value to 6.5 to obtain a mixture;
(4) Naturally cooling the mixture to room temperature, freezing for 12 hours at-20 ℃ in a low-temperature refrigerator, naturally thawing at room temperature, repeatedly freezing and thawing for 3 times, and repeatedly washing the frozen and thawed product with purified water for 4 times;
(5) Freeze-drying the freeze-thaw product at-80 deg.C/24 h, and grinding and sieving the product to obtain dried hydrogel particles with particle size not more than 2 mm.
Example four
A chitosan flaxseed gum cross-linked hydrogel can be applied to the field of gastric bulking agents, and comprises the following steps:
(1) According to the mass ratio of 300:1, weighing 30kg of flaxseed gum and 0.1kg of calcium chloride in mass, continuously stirring for 12 hours at the temperature of 80 ℃, dissolving in purified water, and continuously keeping the temperature at 80 ℃ for standby to obtain a flaxseed gum solution with the mass fraction of 10%;
(2) Weighing 100kg of chitosan according to a proportion, wherein the average molecular weight of the chitosan is 30kDa, the deacetylation degree range is 80 percent, and dissolving the chitosan into an acetic acid solution with the mass fraction of 1 percent to prepare a chitosan solution with the mass fraction of 5 percent;
(3) Mixing the prepared linseed gum solution and the chitosan solution under the condition of 80 ℃ heat preservation, carrying out homogeneous stirring at the speed of 2000r/min for 30min, dropwise adding a sodium hydroxide solution with the concentration of 0.5mol/L in the process, and adjusting the pH value to 4.5 to obtain a mixture;
(4) Naturally cooling the mixture to room temperature, freezing for 8 hours at-60 ℃ in a low-temperature refrigerator, naturally thawing at room temperature, repeatedly freezing and thawing for 3 times, and repeatedly washing the frozen and thawed product with purified water for 4 times;
(5) Freeze-drying the freeze-thaw product at-80 deg.C/24 h, and grinding and sieving the product to obtain dried hydrogel particles with particle size not more than 2 mm.
EXAMPLE five
A chitosan flaxseed gum cross-linked hydrogel is characterized in that reagents and process parameters used in all the steps are the same as those in the two embodiments, the difference is that in the step (1), the addition amount of calcium chloride is 0.3kg, and the mass ratio of the flaxseed gum to the calcium chloride is 50:1.
example six
The chitosan flaxseed gum cross-linked hydrogel comprises the same steps, reagents and process parameters as those of the two embodiments, and is characterized in that in the step (1), the addition amount of calcium chloride is 0.9kg, and the mass ratio of flaxseed gum to calcium chloride is 50:3.
comparative example 1
The chitosan flaxseed gum cross-linked hydrogel comprises the same steps as the two embodiments in terms of reagents and process parameters, and is characterized in that the addition amount of calcium chloride is 0.
Comparative example No. two
A chitosan flaxseed gum cross-linked hydrogel is prepared by the steps and reagents and process parameters used in the steps are the same as those in the embodiment, and the difference is that the addition amount of the flaxseed gum is 0.
Comparative example No. three
A chitosan flaxseed gum cross-linked hydrogel is prepared by the steps and reagents and process parameters used in the steps are the same as those in the embodiment, and the difference is that the addition amount of flaxseed gum is 5kg, and the addition amount of calcium chloride is 2kg.
Comparative example No. four
A chitosan flaxseed gum cross-linked hydrogel is prepared by the steps and reagents and process parameters used in the steps are the same as those in the two examples, and the difference is that in the step (1), the average molecular weight of chitosan is 200kDa, and the deacetylation degree range is 95%.
Comparative example five
The chitosan linseed glue cross-linked hydrogel comprises the same steps, reagents and process parameters as those of the two embodiments, and is characterized in that in the step (1), the average molecular weight of chitosan is 80kDa, and the deacetylation degree range is 50 percent.
Performance test
1. Swelling experiment
1) Configuration of the liquid medium: the artificial gastric juice, the diluted artificial gastric juice, the artificial small intestine juice and the artificial colon juice are prepared according to the provisions of 'Chinese pharmacopoeia' 2020 edition.
Artificial gastric juice: taking 16.4ml of dilute hydrochloric acid, adding about 800ml of water and 10g of pepsin, shaking uniformly, adding water to dilute to 1000ml, and finally, the pH value is about 1.5.
Diluting the artificial gastric juice: taking 100ml of the prepared artificial gastric juice, adding water to dilute the artificial gastric juice into 1000ml of the artificial gastric juice, and finally, the pH value is about 2.5-3.
Artificial small intestine liquid: taking 6.8g of monopotassium phosphate, adding 500ml of water for dissolving, and adjusting the pH value to 6.8 by using 0.1mol/L sodium hydroxide solution; taking 10g of pancreatin, adding a proper amount of water for dissolving, mixing the two solutions, and adding water for diluting to 1000ml.
Artificial colon liquid: 5.59g of dipotassium phosphate and 0.41g of monopotassium phosphate are taken, water is added to dissolve the mixture to 1000ml, and 0.1mol/L sodium hydroxide solution is used for adjusting the pH value to 8.4.
2) The experimental steps are as follows:
s1, accurately weighing 0.500 +/-0.005 g of the hydrogel particles of the above examples 1-6 and comparative examples 1-5 respectively, recording as W dry, then putting each sample into a flask filled with 500ml of diluted artificial gastric juice, and continuously stirring by using a magnetic stirrer under the heating condition of water bath at 37 ℃; carrying out suction filtration to separate a hydrogel sample after swelling for 30min, putting the hydrogel sample into a flask filled with 500ml of diluted artificial gastric juice, continuously stirring for 90min by using a magnetic stirrer under the water bath heating condition of 37 ℃, carrying out suction filtration to obtain the hydrogel sample swollen in the artificial gastric juice, accurately weighing and recording as W Stomach (stomach)
S2, putting the hydrogel sample swollen in the artificial gastric juice in the S1 into a flask filled with 500ml of artificial small intestine solution, and continuously stirring by using a magnetic stirrer under the water bath heating condition of 37 ℃; after the hydrogel swells for 90min, obtaining a hydrogel sample swollen in the artificial small intestine fluid by suction filtration, and accurately weighing and recording as W Small intestine
S3, putting the hydrogel sample swelled in the artificial small intestine solution in the S2 into a flask filled with 500ml of the artificial colon solution, and continuously stirring by using a magnetic stirrer under the water bath heating condition at 37 ℃; after the hydrogel swells for 90min, obtaining a hydrogel sample swollen in the artificial colon fluid by suction filtration, and accurately weighing and recording as W Colon
3) The swelling ratio of the hydrogel was calculated and the results are shown in table 1:
swelling ratio Q of hydrogel in artificial gastric juice Stomach (stomach) =W Stomach (stomach) /W Dry matter
Swelling ratio Q of hydrogel in artificial small intestine liquid Small intestine =W Small intestine /W Dry matter
Swelling ratio Q of hydrogel in artificial colon fluid Colon =W Colon /W Dry food
TABLE 1-hydrogel particle swelling ratios of examples 1-6 and comparative examples 1-5
Item Q Stomach (stomach) Q Small intestine Q Colon
Example 1 42.43 24.65 1.34
Example 2 61.31 29.37 2.64
Example 3 55.53 32.48 3.12
Example 4 45.34 38.57 3.89
Example 5 53.61 26.97 2.59
Example 6 56.28 27.55 2.84
Comparative example 1 22.15 10.46 3.42
Comparative example 2 4.57 3.94 3.24
Comparative example 3 10.64 8.41 2.19
Comparative example 4 11.38 7.56 1.54
Comparative example 5 23.55 16.38 3.24
The detection results of the examples 1 to 6 in the table 1 show that the chitosan flaxseed gum cross-linked hydrogel as a gastric filler has a swelling ratio of more than 40 in simulated gastric fluid and a swelling ratio of more than 20 in simulated intestinal fluid, and the hydrogel basically collapses and only a small amount of residual substances remain in the simulated colonic fluid, so that the chitosan flaxseed gum cross-linked hydrogel has pH sensitivity and a higher swelling ratio in acidic gastric fluid, and the hydrogel collapses and stays and empties in the stomach at different normal physiological times after entering an alkaline colonic environment, so that the chitosan flaxseed gum cross-linked hydrogel is removed after achieving a satiety function, does not produce secondary products, and is harmless to body organs.
Combining the detection results of example 2 and comparative examples 1-3 in table 1, it can be seen that the flaxseed gum is mainly composed of neutral polysaccharide and acidic polysaccharide, the neutral polysaccharide units are mainly xylose, L-arabinose and galactose, and the acidic polysaccharide units are mainly L-rhamnose, D-galacturonic acid, L-galactose and L-fucose, carboxyl groups contained in the flaxseed gum can interact with ammonium ions generated when chitosan is dissolved in an acidic solution electrostatically to form physical crosslinking sites, and the galacturonic acid contained in the flaxseed gum is located in the main chain of the molecule and can contact with calcium ions in calcium chloride to generate bridging action, so that a three-dimensional network can be formed, and the hydrogel can absorb water in gastric acid and expand rapidly.
Combining the detection results of example 2 and comparative examples 4-5 in table 1, it can be seen that, since the solubility of chitosan is determined by the deacetylation degree and the average molecular weight, and the higher the deacetylation degree and the lower the average molecular weight, the better the solubility of chitosan and the faster the dissolution rate, the selection of the deacetylation degree and the average molecular weight of chitosan in the present application can realize the fast crosslinking of the three-dimensional network structure of the chitosan hydrogel, improve the pH sensitivity of the hydrogel, and increase the swelling ratio of the hydrogel in gastric juice.
2. Animal experiments with the application of chitosan flaxseed gum cross-linked hydrogel in gastric bulking agents:
to verify the effectiveness of the hydrogel gastric bulking agent of the present invention, the sample prepared in example 2 was used for feeding and observation of mice tested using KM strain, SPF grade from guangzhou university of traditional Chinese medicine.
Test subjects: male mice of 4 weeks of age were selected, and the initial body weight was about (15.5. + -. 0.3) g, for a total of 10 mice.
The test process comprises the following steps: after the mice were fed with normal feed (10% fat, 70% carbohydrate, 20% protein) for one week, the weight was weighed and randomly divided into test groups and control groups, 10 mice per group. Wherein the test group was fed with high fat diet (fat 45%, carbohydrate 35%, protein 20%), and intragastrically administered with a hydrogel gastric bulking agent dose of 0.5 g/kg-d mixed with 1.0 g/kg-d purified water; the control group was given ordinary feed and gavage was performed with 1.5 g/kg. D purified water.
The experiment was carried out for 8 weeks, all mice had free access to water and food, the weights were weighed once a week, after the intervention, the mice were sacrificed after fasting for 12 hours without water deprivation, and fresh EDTA was collected for anticoagulation and centrifugation for use. The indexes of triglyceride, blood sugar, cholesterol, low density cholesterol and high density cholesterol in the blood sample are measured by using a Roche cobasC702 full-automatic biochemical analyzer, and the detection results are shown in tables 2-3.
TABLE 2 average body weight statistics of mice in the control group and the test group of example 2 over 8 weeks
Figure BDA0003514595050000101
TABLE 3 Biochemical index of blood samples of control and test groups of mice of example 2
Biochemical index of blood Test group Control group
Blood sugar value (mmol/L) 6.49±0.14 8.12±0.11
Triglyceride (mmol/L) 0.68±0.05 0.75±0.10
Cholesterol(mmol/L) 3.11±0.16 3.53±0.12
High density cholesterol (mmol/L) 1.07±0.13 1.49±0.21
Low density cholesterol (mmol/L) 1.67±0.13 1.86±0.12
According to the test results in tables 2-3, the body weight and the final biochemical index value of the blood sample of the mice in the test group fed with the high-fat feed are still lower than those of the mice in the control group, which indicates that the chitosan flaxseed gum crosslinked hydrogel can effectively inhibit the increase of the body weight, blood fat, blood sugar and other indexes of the mice when being used as a gastric bulking agent, and has the physiological functions of losing weight and reducing fat and regulating the body weight.
The above-mentioned embodiments are provided to further explain the objects, technical solutions and advantages of the present invention in detail, and it should be understood that the above-mentioned embodiments are only examples of the present invention and are not intended to limit the scope of the present invention. It should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The chitosan flaxseed gum crosslinked hydrogel is characterized by comprising the following components in parts by weight: and (3) chitosan: 100 parts of (A); flaxseed gum: 10-30 parts; calcium salt: 0.1-1 part, wherein the average molecular weight of the chitosan is 30-100 kDa, and the deacetylation degree is 80-100 percent.
2. The chitosan flaxseed gum cross-linked hydrogel of claim 1, wherein said calcium salt is one or more of calcium chloride, calcium gluconate, calcium lactate and calcium hydrogen phosphate.
3. The chitosan flaxseed gum cross-linked hydrogel of claim 1, comprising the following components in parts by weight: and (3) chitosan: 100 parts of (A); flaxseed gum: 15-20 parts of a stabilizer; calcium salt: 0.3 to 0.6 portion.
4. The chitosan flaxseed gum cross-linked hydrogel of claim 1, wherein said calcium salt is calcium chloride, and the mass ratio of flaxseed gum to calcium chloride is 25:1.
5. a method for preparing a chitosan linseed gum cross-linked hydrogel, which is used for preparing the chitosan linseed gum cross-linked hydrogel according to any one of claims 1 to 4, and which comprises the steps of:
(1) Mixing flaxseed gum with calcium salt under heat preservation, and dissolving in pure water to obtain flaxseed gum solution; dissolving chitosan in an organic acid aqueous solution to prepare a chitosan solution;
(2) Mixing the premixed solution and the chitosan solution under the condition of heat preservation, uniformly stirring, and dropwise adding an alkali solution to adjust the pH value to obtain a mixture;
(3) And cooling the mixture, freezing, repeatedly freezing and thawing, cleaning and drying to obtain the hydrogel particles.
6. The method for preparing a chitosan flaxseed gum cross-linked hydrogel according to claim 5, wherein in the step (1), the chitosan solution has a mass fraction of 5% -10%, and the organic acid aqueous solution has a volume fraction of 0.5% -2% of acetic acid aqueous solution.
7. The method for preparing a chitosan flaxseed gum cross-linked hydrogel according to claim 5, wherein in the step (1), the mass fraction of the flaxseed gum in the flaxseed gum solution is 5% -10%.
8. The process for preparing a chitosan flaxseed gum cross-linked hydrogel as claimed in claim 5, wherein in the step (2), the pH is adjusted to 4.5-6.5.
9. The method for preparing the chitosan flaxseed gum cross-linked hydrogel according to claim 5, wherein in the step (1), the temperature is kept at 80-90 ℃, and the mixing and stirring time is 6-12h; in the step (3), the temperature of the freezing treatment is-60 ℃ to-20 ℃ for 6-125h, and the freezing and thawing are repeated for 1-3 times.
10. Use of a chitosan flaxseed gum cross-linked hydrogel according to any one of claims 1 to 4 in a gastric bulking agent.
CN202210162581.3A 2022-02-22 2022-02-22 Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent Active CN115154407B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210162581.3A CN115154407B (en) 2022-02-22 2022-02-22 Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210162581.3A CN115154407B (en) 2022-02-22 2022-02-22 Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent

Publications (2)

Publication Number Publication Date
CN115154407A true CN115154407A (en) 2022-10-11
CN115154407B CN115154407B (en) 2023-04-18

Family

ID=83476180

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210162581.3A Active CN115154407B (en) 2022-02-22 2022-02-22 Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent

Country Status (1)

Country Link
CN (1) CN115154407B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117530929A (en) * 2024-01-10 2024-02-09 东华大学 Weight-losing capsule

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001316271A (en) * 2000-05-01 2001-11-13 Kobayashi Pharmaceut Co Ltd Chitosan containing composition
US20080095911A1 (en) * 2004-12-08 2008-04-24 Sarah Adams Satiety Enhancing Food Product And A Method For Manufacturing Such
WO2008068762A2 (en) * 2006-12-07 2008-06-12 Noah Ben-Shalom Chitosan formulation for cholesterol reduction in humans
US20140099371A1 (en) * 2012-10-05 2014-04-10 China Medical University Medicinal carriers, and preparation method and uses thereof
CN106478963A (en) * 2016-10-11 2017-03-08 中国农业科学院油料作物研究所 Flaxseed gum/cellulose composite aquogel and preparation method thereof
CN106750398A (en) * 2016-11-25 2017-05-31 暨南大学 Carry medicine shitosan/dual cross-linked hydrogel of sodium alginate and its preparation method and application
US20210085823A1 (en) * 2015-12-18 2021-03-25 Oceanit Laboratories, Inc. Methods of making chitosan/hyaluronic acid hydrogel compositions and compositions made therefrom

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001316271A (en) * 2000-05-01 2001-11-13 Kobayashi Pharmaceut Co Ltd Chitosan containing composition
US20080095911A1 (en) * 2004-12-08 2008-04-24 Sarah Adams Satiety Enhancing Food Product And A Method For Manufacturing Such
WO2008068762A2 (en) * 2006-12-07 2008-06-12 Noah Ben-Shalom Chitosan formulation for cholesterol reduction in humans
US20140099371A1 (en) * 2012-10-05 2014-04-10 China Medical University Medicinal carriers, and preparation method and uses thereof
US20210085823A1 (en) * 2015-12-18 2021-03-25 Oceanit Laboratories, Inc. Methods of making chitosan/hyaluronic acid hydrogel compositions and compositions made therefrom
CN106478963A (en) * 2016-10-11 2017-03-08 中国农业科学院油料作物研究所 Flaxseed gum/cellulose composite aquogel and preparation method thereof
CN106750398A (en) * 2016-11-25 2017-05-31 暨南大学 Carry medicine shitosan/dual cross-linked hydrogel of sodium alginate and its preparation method and application

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117530929A (en) * 2024-01-10 2024-02-09 东华大学 Weight-losing capsule

Also Published As

Publication number Publication date
CN115154407B (en) 2023-04-18

Similar Documents

Publication Publication Date Title
Yang et al. Characterization of insoluble dietary fiber from three food sources and their potential hypoglycemic and hypolipidemic effects
CN106478825B (en) Method for preparing oxidized cellulose for hemostasis in ramie oxidation degumming process
CN115154407B (en) Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent
CN111732741B (en) Method for crosslinking hyaluronic acid and epsilon-polylysine, composite crosslinked product obtained by method and application of composite crosslinked product
Che Nan et al. Preparation and Swelling Study of CMC Hydrogel as Potential Superabsorbent.
CN112262984B (en) Hydrogel for assisting in diet control and preparation method and application thereof
CN107141519B (en) A kind of modification of chitosan base superabsorbent hydrogel and its preparation and application
Mahmoud Nasef et al. Preparation and properties of non-crosslinked and ionically crosslinked chitosan/agar blended hydrogel films
US20040215005A1 (en) Chitosan preparation
CN111269437A (en) Preparation method of composite hydrogel with self-healing property and adhesion property
CN114366756B (en) Crosslinked chitosan hydrogel stomach filler and preparation method and application thereof
Adekanmi et al. Different processing sequential protocols for extraction, quantification and characterization of chitosan from cray fish
US4575519A (en) Porous chitin shaped article and production thereof
CN111303492B (en) Waterproof ultra-light plant fiber composite material applied to degradable dinner plate and preparation method thereof
CN112106976A (en) Preparation method of minced fillet product additive rich in modified nano-cellulose
CN114098050B (en) Lignan hydrogel based on soy protein isolate and carrageenan and preparation method thereof
JP2766829B2 (en) Partially gelled hydrophilic mannan paste-like food material and its production method
US20180057614A1 (en) Depolymerisation of alginic acid
CN106589441A (en) Preparation method for water absorbent with high strength and high water absorption rate
CN111675773B (en) Preparation method and application of chitosan with controllable molecular weight range
CN116421771B (en) Novel porous starch hemostatic powder and preparation method and application thereof
JPH11243876A (en) Gelling agent and jelly-like material
CN114702701B (en) Xanthan gum agar composite derivative, and preparation method and application thereof
CN117024673A (en) Super absorbent polymer and preparation method thereof
CN116376118A (en) Radix puerariae starch/montmorillonite antibacterial composite membrane and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
TA01 Transfer of patent application right

Effective date of registration: 20220929

Address after: No. 583, Zone C, Second Floor, College Park, Zhongguancun Dongsheng Science Park, No. A18 Xueqing Road, Haidian District, Beijing 100190

Applicant after: Beijing Hualiang Engine Network Technology Co.,Ltd.

Address before: 301706 room 127, No. 3, Xingfu Road, dajianchang Town, Wuqing District, Tianjin

Applicant before: Youdao (Tianjin) Health Consulting Co.,Ltd.

TA01 Transfer of patent application right
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant