CN111393677A - Preparation method of nano composite hydrogel for rapid blood coagulation promotion - Google Patents
Preparation method of nano composite hydrogel for rapid blood coagulation promotion Download PDFInfo
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- CN111393677A CN111393677A CN202010353209.1A CN202010353209A CN111393677A CN 111393677 A CN111393677 A CN 111393677A CN 202010353209 A CN202010353209 A CN 202010353209A CN 111393677 A CN111393677 A CN 111393677A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention provides a preparation method of a nano composite hydrogel for rapid blood coagulation promotion, belonging to the technical field of medical auxiliary materials. The blood coagulant which can be applied to the vacuum blood collection tube is prepared by utilizing an electron beam radiation crosslinking technology to carry out radiation crosslinking reaction on natural polysaccharide, blood coagulation factors and the like. The method has the advantages of capability of shortening the hemagglutination and coagulation time, no influence on biochemical detection indexes, no toxicity, mild reaction conditions, no addition of a cross-linking agent in the reaction process, easy storage and the like.
Description
Technical Field
The invention belongs to the technical field of medical auxiliary materials, and relates to a preparation method of a nano composite hydrogel for rapid blood coagulation promotion.
Background
The medical inspection technology is now in the new era of full automation and microcomputer management, and is in the field of clinical inspection, no matter in clinical chemistry, serology, immunology and other detection. Most of the samples used require serum isolation. How to separate serum rapidly and sufficiently and simplify the operation is a problem which needs to be solved urgently by the medical inspection community. In addition, most clinical indexes such as biochemistry, immunity and the like use serum samples, while an isolated blood sample generally needs about 1 hour from coagulation to serum exudation, and the serum sample is a precondition for improving the inspection efficiency and accuracy in order to quickly obtain high-quality serum. The effective application of the rapid blood coagulant in the vacuum blood collection tube can effectively shorten the blood coagulation time, improve the serum separation efficiency and rapidly and accurately obtain the relevant results of biochemical test and immunoassay.
Chinese patent No. 104101522A describes a composite blood coagulation promoting powder composed of coagulant, adsorbent, stabilizer, fixative, blood cell wall removing agent, and anti-fibrinolytic agent, which can be used in vacuum blood collection tubes or other non-vacuum blood collection tubes by using alcohol, isopropanol, water, etc. as solvent to prepare suspension. The patent technology has the characteristics of good procoagulant effect, easy storage, low-temperature hemolysis prevention and the like. However, the thrombin component described in this patent is thrombin, and thus, a special apparatus is required for the detection, which is disadvantageous in that the cost investment is high. Further, chinese patent 102212514a describes a blood coagulant for blood collection containers, which is characterized in that the blood coagulant is composed of a blood adhesion preventing agent, thrombin, phosphatidylethanolamine, fine silica powder and ethanol, and can be used in vacuum blood collection tubes or other non-vacuum blood collection tubes. The phosphatidylethanolamine and the silicon dioxide micropowder which are described in the patent are used together, so that blood coagulation can be promoted, fibrin filaments can be avoided, the sample storage time is long, the blood coagulation speed is slightly influenced by temperature, and the biochemical and immune experiment detection indexes including ions are not influenced. In addition, the blood sampling tube is not influenced by the material of the blood sampling tube, and no hemolysis phenomenon is caused by the glass tube or the plastic tube. The longest blood coagulation time is the biggest defect of the patent.
A hydrogel is a three-dimensional or interpenetrating network between a liquid and a solid, a hydrophilic polymer gel that swells significantly in water, but is insoluble in water. The invention utilizes radiation technology to effectively compound the nano coagulation promoting factor and the hydrogel carrier, and utilizes the strong water absorbability of the dry powder particles to enhance the effect of the nano coagulation promoting factor on blood coagulation. This vacuum test tube makes the blood of gathering solidify in 3 minutes, does not arouse the hemolysis, stops fibrin silk's formation, need not special check out test set, and the material of vacuum test tube does not influence the hemolysis, easily stores, is expected to be applied to vacuum test tube and is managed or non-vacuum test tube.
Compared with a chemical preparation method, the radiation technology realizes effective supplement and perfection, and the specific expression is that no substance toxic to human bodies is required to be added in the ① reaction process, the crosslinking degree is high, the hydrogel purity is high, the reaction condition ② is mild and can be carried out at room temperature, ③ can accurately regulate and control the microstructure and the water absorption performance of the hydrogel by controlling the polymer components and the radiation condition, the preparation, shaping and sterilization processes of the ④ hydrogel can be synchronously completed, and the economic cost for preparing the hydrogel by using the radiation technology is lower in comprehensive and long-term view.
The invention aims to solve the problem of disclosing a preparation method of a nano composite hydrogel for rapidly accelerating blood coagulation so as to overcome the defects in the prior art.
Disclosure of Invention
The invention aims to provide a preparation method of a nano composite hydrogel for rapidly accelerating blood coagulation aiming at the problems in the prior art, and the technical problem to be solved by the invention is how to prepare a hydrogel-based blood coagulation accelerator by taking natural polysaccharide as a main raw material.
The purpose of the invention can be realized by the following technical scheme: the preparation method of the nano composite hydrogel for rapidly accelerating blood coagulation is characterized by comprising the following steps:
① mixing 0.01-1 g coagulant, 7-100 g adsorbent, 0.15-5 g blood cell wall removing agent and 0.15-5 g anti-fibrinolytic agent uniformly, drying at a temperature not exceeding 100 ℃;
② preparing natural polysaccharide into water solution, stirring for 0.5-2 h to form uniform polymer solution;
③ dispersing the coagulant powder dispersion system obtained in step ① into the natural polysaccharide solution obtained in step ②, spreading the mixed solution in a glass dish to a thickness of 2-4 mm, rapidly and circularly freezing and thawing for 3-5 times, and storing in a 4 deg.C freezer for use;
④, placing the sample obtained in the step ③ under an electron beam for radiation crosslinking reaction, wherein the selected electron beam energy is 1-5 MeV, the radiation dose is 4-40 kGy, the dose rate is 4-20 kGy/pass, and the final product is the rapid blood coagulation promoting nanocomposite hydrogel.
The natural polysaccharide is one or more of chitosan and derivatives thereof, cellulose and derivatives thereof, sodium alginate and the like. One or more natural polysaccharides can be subjected to self-crosslinking or mutual crosslinking in the irradiation process, so that the hydrogel is ensured to have a certain network structure, and the water absorption performance of the hydrogel is further enhanced.
The coagulant is one or more of thrombin, phosphate ethanolamine, wedelolactone and the like.
The adsorbent is calcium carbonate, quartz powder, white carbon black, talcum powder and SiO2And the like.
The blood cell wall removing agent is one or more of glycine, polydimethylsiloxane, tween 80 and the like.
The fibrinolytic agent is one or more of tranexamic acid, aminocaproic acid, aprotinin and the like.
The beneficial effects are that:
1. the radiation technology is non-toxic, the reaction condition is mild, no cross-linking agent, initiator and any substance toxic to human bodies are added in the reaction process, and secondary pollution can be effectively avoided.
2. The rapid coagulation of blood is realized, the hemolysis phenomenon and the formation of fibrin filaments are avoided, the high-quality separation efficiency of large-volume serum can be realized, and the rapid coagulation accelerating effect of blood is good.
3. The nano composite hydrogel product for accelerating blood coagulation quickly appears as powder and is easy to transport and store.
4. The effective preparation of the compound solvent preparation is beneficial to production and cost saving.
5. The coagulant can be prepared into suspension with water, ethanol and the like according to a certain proportion, sprayed on the wall of a vacuum blood collection vessel, can directly act with blood, shortens the blood coagulation time, and does not influence biochemical detection indexes.
6. The product can solidify the collected blood within 3 minutes, does not need special inspection equipment, does not influence hemolysis by the material of the used vacuum blood collection tube, is easy to store, and is particularly suitable for the clinical treatment fields of rapid high-quality biochemical inspection, immune inspection and the like.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Example 1:
phosphate Ethanolamine (0.01g), 30nm SiO was weighed2(7g) Uniformly mixing polydimethylsiloxane (0.15g) and tranexamic acid (0.15g), dissolving the mixture in an ethanol solution of 50m L, filtering and drying to obtain the blood coagulation promoting powder, doping the blood coagulation promoting powder into an ethanol solution of carboxymethyl chitosan and sodium alginate (1:4) according to the mass fraction of 2%, paving the mixture in a glass dish of 90mm, wherein the thickness is about 2-4 mm, quickly and circularly freezing and unfreezing the mixture for 3-5 times, storing the mixture in a freezer at 4 ℃ for later use, placing an obtained sample under an electron beam for radiation crosslinking reaction, selecting the electron beam energy of 1MeV, the radiation dose of 4kGy and the dose rate of 4kGy/pass, and finally obtaining the product, namely the blood rapidly-procoagulated nano composite hydrogelHemolysis and fibrin thread formation.
Example 2:
weighing 0.1g of wedelolactone, 10g of white carbon black, 800.2g of tween and 0.15g of aminocaproic acid, uniformly mixing, dissolving in a water solution of 50m L, filtering and drying to obtain blood coagulation promoting powder, doping the blood coagulation promoting powder into a carboxymethyl chitosan and carboxymethyl cellulose (1:3) water solution according to the mass fraction of 2%, paving the mixture into a 90mm glass dish to obtain a glass dish with the thickness of about 2-4 mm, quickly and circularly freezing and unfreezing for 3-5 times, storing the glass dish in a freezer at 4 ℃ for later use, placing an obtained sample in an electron beam for radiation crosslinking reaction, selecting the electron beam energy of 1MeV, the radiation dose of 20kGy and the dose rate of 10kGy/pass, and finally obtaining the product, namely the quick-coagulation promoting nano hydrogel.
Example 3:
weighing 0.5g of thrombin, 50g of calcium carbonate, 2.5g of glycine and 2.5g of aminocaproic acid, uniformly mixing, dissolving in 50m L ethanol solution, filtering and drying to obtain the blood coagulation promoting powder, doping the blood coagulation promoting powder into the ethanol solution of carboxymethyl cellulose and sodium alginate (1:2) according to the mass fraction of 2%, paving the mixture into a 90mm glass dish, quickly and circularly freezing and unfreezing for 3-5 times at the thickness of about 2-4 mm, and storing the glass dish in a freezing cabinet at 4 ℃ for later use.
Example 4:
weighing 0.8g of phosphate ethanolamine and wedelolactone (1:1) in total, 80g of talcum powder, 3g of polydimethylsiloxane and 3g of aprotinin, uniformly mixing, dissolving in 50m L ethanol solution, filtering and drying to obtain blood procoagulant powder, doping the powder into starch and carboxymethyl chitosan (1:3) hydrogel solution according to the mass fraction of 2%, spreading the solution into a 90mm glass dish, quickly and circularly freezing and thawing for 3-5 times at the thickness of 2-4 mm, and storing in a 4 ℃ freezer for later use, placing a sample obtained in the step ③ in an electron beam for radiation crosslinking reaction, wherein the selected electron beam energy is 1MeV, the radiation dose is 40kGy, the dose rate is 10kGy/pass, and the finally obtained product is the quick procoagulant nano hydrogel.
Example 5:
weighing 1g of phosphoethanolamine, 100g of quartz powder, 5g of dimethyl siloxane, Tween 80(1:1), 5g of tranexamic acid and aprotinin (1:1), uniformly mixing, dissolving in 50m L ethanol solution, filtering and drying to obtain the blood procoagulant powder, doping the blood procoagulant powder into carboxymethyl chitosan and carrageenan (1:1) hydrogel solution according to the mass fraction of 2%, spreading the mixture to a 90mm glass dish, quickly circulating and freezing and thawing for 3-5 times with the thickness of about 2-4 mm, placing the glass dish in a freezer at 4 ℃ for storage, placing the sample obtained in the step ③ under an electron beam for radiation crosslinking reaction, selecting the electron beam energy of 1MeV, the radiation dose of 40kGy and the dose rate of 20kGy/pass, and finally obtaining the product, namely the quick procoagulant nano hydrogel.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (6)
1. The preparation method of the nano composite hydrogel for rapidly accelerating blood coagulation is characterized by comprising the following steps:
① mixing 0.01-1 g coagulant, 7-100 g adsorbent, 0.15-5 g blood cell wall removing agent and 0.15-5 g anti-fibrinolytic agent uniformly, drying at a temperature not exceeding 100 ℃;
② preparing natural polysaccharide into water solution, stirring for 0.5-2 h to form uniform polymer solution;
③ dispersing the coagulant powder dispersion system obtained in step ① into the natural polysaccharide solution obtained in step ②, spreading the mixed solution in a glass dish to a thickness of 2-4 mm, rapidly and circularly freezing and thawing for 3-5 times, and storing in a 4 deg.C freezer for use;
④, placing the sample obtained in the step ③ under an electron beam for radiation crosslinking reaction, wherein the selected electron beam energy is 1-5 MeV, the radiation dose is 4-40 kGy, the dose rate is 4-20 kGy/pass, and the final product is the rapid blood coagulation promoting nanocomposite hydrogel.
2. The method for preparing the nanocomposite hydrogel for rapidly accelerating blood coagulation according to claim 1, wherein the natural polysaccharide is one or more of chitosan and derivatives thereof, cellulose and derivatives thereof, sodium alginate and the like.
3. The method for preparing the nanocomposite hydrogel for rapidly accelerating blood coagulation according to claim 1 or 2, wherein the coagulant is one or more of thrombin, phosphate wedelolactone, deltoid lactone and the like.
4. The method for preparing the nano-composite hydrogel for rapidly accelerating blood coagulation according to claim 3, wherein the adsorbent is calcium carbonate, quartz powder, white carbon black, talcum powder or SiO2And the like.
5. The method for preparing the nanocomposite hydrogel for rapidly procoagulant blood according to claim 3, wherein the blood cell wall removing agent is one or more of glycine, polydimethylsiloxane, Tween 80 and the like.
6. The method for preparing the nanocomposite hydrogel for rapidly accelerating blood coagulation according to claim 3, wherein the anti-fibrinolytic agent is one or more of tranexamic acid, aminocaproic acid, aprotinin and the like.
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