CN102228716A - Collagen-polycaprolactone (PCL) dental hemostatic sponge and preparation method thereof - Google Patents

Collagen-polycaprolactone (PCL) dental hemostatic sponge and preparation method thereof Download PDF

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Publication number
CN102228716A
CN102228716A CN2011101732910A CN201110173291A CN102228716A CN 102228716 A CN102228716 A CN 102228716A CN 2011101732910 A CN2011101732910 A CN 2011101732910A CN 201110173291 A CN201110173291 A CN 201110173291A CN 102228716 A CN102228716 A CN 102228716A
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China
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pcl
collagen protein
dentistry
collagen
sthptic sponge
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CN2011101732910A
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Chinese (zh)
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穆畅道
张云凤
谭欢
李德富
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Sichuan University
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Sichuan University
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Abstract

The invention provides a collagen-polycaprolactone (PCL) dental hemostatic sponge and a preparation method thereof. The method comprises the following steps of: blending 0.2 to 1 mass percent of collagen solution and 0.5 to 10 mass percent of PCL solution, stirring at the temperature of between 1 and 30DEG C, reacting for 1 to 6 hours to obtain complex liquid; adding auxiliaries into the complex liquid, continuously stirring at the temperature of between 1 and 30DEG C for 1 to 4 hours to obtain a mixed solution; pouring the mixed solution into a mold, freezing at the temperature of -20DEG C for 0.5 to 4 hours; and performing freeze drying in a freezer dryer to obtain the collagen-PCL hemostatic sponge. The collagen-PCL hemostatic sponge prepared by the method has good retention ability, hemostasia, anti-inflammatory and antibacterial property and biocompatibility, is effective and safe without toxic or side effect, can be widely used as a postoperative hemostatic material for exodontias and other oral surgeries and has good market application prospect; and waste can be degraded and cannot pollute environment.

Description

A kind of collagen protein-PCL dentistry sthptic sponge and preparation method thereof
Technical field
The present invention relates to the medical material preparing technical field, in particular to a kind of collagen protein-PCL dentistry sthptic sponge and preparation method thereof with favorable mechanical performance, maintenance, degradability and better hemostatic, anti-inflammatory, biocidal property, biocompatibility and biodegradability.
Background technology
Present clinical odontopathy patient's number is on the increase, and the patient relates to child, youth, mid-aged population.Extraction is one of common operation of the department of stomatology, and the exodontia postoperative hemorrhage is an exodontia back common complication.The hemostasis method mainly contains compression method, sewing, packing etc. after the Chang Yong extraction clinically, and wherein compression method is the most frequently used traditional hemostasis method.As: application contains YUNNAN BAIYAO antiseptic gauze lap and simple antiseptic gauze lap local compression is had tooth pulled out wound surface to reach the hemostasis purpose.But the method for cotton balls or gauze ball hemostasis by compression has following shortcoming and defect: it is longer to reach thorough hemostasis required time; Cotton yarn can carry out hemostasis by compression to less hemorrhage of the back gingiva wound surface of having tooth pulled out, but to big wound surface anthemorrhagic difficulty, must be in conjunction with styptic powder and hemorrhage, or wound surface is sewed up hemostasis handle; In addition, the cotton yarn hemostasis only is a physics hemostasis method, can not play healing effect etc. to wound surface.In this case, research and development have good maintenance and hemostasis and pain-relieving, antiinflammatory and bacteriostatic functions and hemostatic material easy to use extremely urgent.
In recent years, more hemostatic material constantly is introduced in alveolus surgery.As modification hemostatic gauze, dentistry tampon etc.Wherein, it is main raw material(s) that the modification hemostatic gauze adopts medical absorbent cotton/gauze, adopts the technology and the technology of innovation, and natural fiber is made through controlled micro crystallization processing and cross-linking reaction, and this modification gauze has good water-solubility and salt dissolubility, and certain anastalsis is arranged.But gauze has the characteristics of light weight and causes that this material is easy to emersion, retention effect is poor, makes it not ideal enough in actual applications, and this hemostatic gauze does not have the antiinflammatory bacteriostasis simultaneously, can not prevent to infect in the tooth socket.
The spirality fiber shape protein that collagen protein is made up of 3 peptide chains, it has extremely low antigenicity and high degradability, bioresorbable, and has certain hemostatic function and promote the function that cell is grown.Collagen protein and modified product thereof are used for the production of biological dressing in a large number.But collagen protein itself has bad mechanical property and the fast shortcoming of degradation speed, has limited its application.Therefore, to carry out modification to collagen protein usually, to improve the performance of collagen protein materialization aspect.With collagen protein and other macromolecular material blend is one of method of modifying of using always, and blending and modifying can improve the intensity of collagen protein by secondary bonds such as hydrogen bonds, and has increased the advantageous property that many collagen protein do not have.Polycaprolactone (PCL) is a kind of synthetic family macromolecule polymer, has advantages such as good biocompatibility, nontoxic, biodegradable.PCL is a lyophobic dust, and the collagen protein dissolution velocity that can slow down, thereby prolong drug release time are a kind of ideal collagen-modified dose.
The present invention adopts PCL and the collagen blending with certain intensity and hardness, and lyophilizing prepares mandruka at low temperatures.The collagen protein of gained-PCL sthptic sponge also has certain degree of hardness and intensity except the advantage that hemostatic material commonly used is arranged, maintenance is good in the time of hemostasis by compression, is difficult for emersion.The auxiliary additive thrombin is different from other hemorrhage among the present invention, does not need the clotting mechanism of mediator behind general metabolism, be used for wound surface after, solidifying of accelerate blood reaches the hemostatic purpose.Sthptic sponge provided by the invention has in addition added antiinflammatory antipathogenic compositions such as tea polyphenols, chitosan, can suppress common periodontal pathogenic bacterium growth when being used as the local hemostasis material of having tooth pulled out hemorrhage, and prevention infection takes place.Therefore, use collagen protein-PCL sthptic sponge can reach anastalsis and energy prevention infection preferably after the extraction.
Summary of the invention
Normal gauze as extraction after dental filling material, its anthemorrhagic performance is poor, stationarity is low and material itself does not almost have antiinflammatory and bacteriostatic functions, can not satisfy the handling characteristics of hemostatic material after the extraction preferably.The invention provides a kind of collagen protein-PCL dentistry sthptic sponge and preparation method thereof with favorable mechanical performance, heat stability, degradability and certain hemostasis and pain-relieving, antiinflammatory and bacteriostatic functions for this reason.
The present invention is achieved through the following technical solutions, and except that specifying, related umber is parts by weight, and percentage ratio is percetage by weight.
The invention provides a kind of collagen protein-PCL dentistry sthptic sponge, the preparation method of this sthptic sponge is specific as follows:
(1) respectively collagen protein and PCL are dissolved in the selected solvent, being mixed with collagen solution and the mass fraction that mass fraction is (0.2 ~ 1) % is the PCL solution of (0.5-10) %, then two kinds of solution are mixed, and, prepare complex liquid in 1 ~ 30 ℃ of stirring reaction of temperature 1 ~ 6 hour;
(2) in above-mentioned complex liquid, add auxiliary additive, continue for 1 ~ 30 ℃ to stir 1 ~ 4 hour, make mixed solution in temperature;
(3) above-mentioned mixed solution is poured in the mould,, placed freezer dryer lyophilizing molding promptly to get collagen protein-PCL dentistry sthptic sponge then in-20 ℃ times freezing 0.5 ~ 4 hour.
In above-mentioned technology case, described solvent is any one or the two kinds of mixture in trifluoroethanol, the hexafluoroisopropanol.
In above-mentioned technology case, the mass ratio of collagen protein and PCL is 1:(4 ~ 20).
In order to reach purpose of the present invention, also needing to add auxiliary additive, described auxiliary additive in the complex liquid is any one or two kinds of mixture in hemorrhage and the antiinflammatory antibacterial.
Described hemorrhage is any one or a few mixture in thrombin, YUNNAN BAIYAO, Radix Notoginseng, Herba Cirsii, Pseudobulbus Bletillae (Rhizoma Bletillae), the Pollen Typhae.
Described antiinflammatory antibacterial is any one or a few mixture in tea polyphenols, chitosan, benzylphenol, the tannin.
In above-mentioned technology case, the weight ratio of auxiliary additive and collagen protein-PCL complex liquid is 1: (200 ~ 2000).
Collagen protein provided by the invention-PCL dentistry sthptic sponge can be used as the antibacterial material of hemostasis, antiinflammatory behind extraction or other the common operation on oral cavity.
Compared with the prior art the present invention has many-sided good effect and advantage, but concrete inductive generalization is as follows:
(1) collagen protein provided by the invention-PCL dentistry sthptic sponge is compared with commonly used gauze or tampon, and good, the easy degraded of maintenance,, no cytotoxicity reaction non-stimulated to body and side effect are as dentistry hemostatic material better effects if;
(2) the auxiliary additive thrombin is different from other hemorrhage among the present invention, does not need the clotting mechanism of mediator behind general metabolism, be used for wound surface after, directly act on the Fibrinogen in the blood, make it to change into fibrin, solidifying of accelerate blood reaches the hemostatic purpose.Thrombin is applied to extraction, and is particularly remarkable to disturbances of blood coagulation person haemostatic effect;
(3) additive that uses among the present invention is natural Chinese medicinal herb such as polysaccharide, polyphenol, and side effect is little when having hemostasis and pain-relieving, antiinflammatory and bacteriostatic functions.After the exodontia this sthptic sponge clogged in tooth socket haemostatic effect better and need not to sew up, and can keep hemostasis, antiinflammatory bacteria resistance function for a long time;
When (4) sthptic sponge provided by the invention is used for postoperative wound surface, do not need again subsidiary any medicine, just can stop blooding rapidly, antiinflammatory, also can suppress courses of infection.Technology of the present invention is easy, effect is obvious, safe and reliable, be worthy of popularization.
The present invention also has some otherwise advantages.
The specific embodiment
Provide three embodiment of the present invention below, the present invention is specifically described by embodiment.Be necessary to be pointed out that at this; embodiment only is used for the present invention is further detailed; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
In following examples, except that specifying, related umber is parts by weight, and percentage ratio is percetage by weight.
Embodiment 1
With mass fraction is that 1% collagen protein trifluoroethanol solution and mass fraction are 4% PCL trifluoroethanol solution according to collagen protein and PCL dry weight than being the ratio blend of 1:4, and 20 ℃ are stirred the complex liquids that obtained collagen protein and PCL in 6 hours down.In auxiliary additive (in tea polyphenols, thrombin dry weight than being the ratio blend of 1:1) and complex liquid weight ratio is that the ratio of 1:400 adds auxiliary additive in the complex liquid of collagen protein and PCL, in 20 ℃ of stirrings 1 hour, be configured to the mixed liquor of collagen protein, PCL and auxiliary additive.With the mixed liquor of collagen protein, PCL and auxiliary additive inject mould in-20 ℃ freezing 2 hours down, be placed at last in the freeze dryer, about-70 ℃, kept about 10 hours down.Then mould is taken out and promptly obtain collagen protein-PCL dentistry sthptic sponge.
Embodiment 2
With mass fraction is that 0.5% collagen protein hexafluoroisopropanol solution and mass fraction are 2.5% PCL hexafluoroisopropanol solution according to collagen protein and PCL dry weight than being the ratio blend of 1:5, and 25 ℃ are stirred the complex liquids that obtained collagen protein and PCL in 5 hours down.In auxiliary additive (in tea polyphenols, chitosan, thrombin, Pseudobulbus Bletillae (Rhizoma Bletillae) dry weight than being the ratio blend of 2:1:2:1) and complex liquid weight ratio is that the ratio of 1:600 adds auxiliary additive in the complex liquid of collagen protein and PCL, in 20 ℃ of stir abouts 2 hours, be configured to the mixed liquor of collagen protein, PCL and auxiliary additive.With the mixed liquor of collagen protein, PCL and auxiliary additive inject mould in-20 ℃ freezing 4 hours down, be placed at last in the freeze dryer, about-70 ℃, kept about 10 hours down.Then mould is taken out and promptly obtain collagen protein-PCL dentistry sthptic sponge.
Embodiment 3
With mass fraction is that 0.5% collagen protein trifluoroethanol solution and mass fraction are 5% PCL trifluoroethanol solution according to collagen protein and PCL dry weight than being the ratio blend of 1:10, and 30 ℃ of following stirring reactions obtained the complex liquid of collagen protein and PCL in 2 hours.In auxiliary additive (in tea polyphenols, benzylphenol and thrombin dry weight than being the ratio blend of 1:1:1) and complex liquid weight ratio is that the ratio of 1:1000 adds auxiliary additive in the complex liquid of collagen protein and PCL, in 30 ℃ of following stir abouts 4 hours, be configured to the mixed liquor of collagen protein, PCL and auxiliary additive.With the mixed liquor of collagen protein, PCL and auxiliary additive inject mould in-20 ℃ freezing 1 hour down, be placed at last in the freeze dryer, about-50 ℃, kept about 15 hours down.Then mould is taken out and promptly obtain collagen protein-PCL dentistry sthptic sponge.

Claims (7)

1. collagen protein-PCL dentistry sthptic sponge is characterized in that preparation method is as follows:
(1) be dissolved in collagen protein and polycaprolactone (PCL) in the solvent respectively, being mixed with collagen solution and the mass fraction that mass fraction is (0.2 ~ 1) % is the PCL solution of (0.5 ~ 10) %, then two kinds of solution are mixed, and, prepare complex liquid in 1 ~ 30 ℃ of stirring reaction of temperature 1 ~ 6 hour;
(2) in above-mentioned complex liquid, add auxiliary additive, and continue for 1 ~ 30 ℃ to stir 1 ~ 4 hour, make mixed solution in temperature;
(3) above-mentioned mixed solution is poured in the mould, in-20 ℃ times freezing 0.5 ~ 4 hour, the lyophilizing molding promptly got collagen protein-PCL dentistry sthptic sponge then.
2. collagen protein according to claim 1-PCL dentistry sthptic sponge is characterized in that described solvent is any one or the two kinds of mixture in trifluoroethanol, the hexafluoroisopropanol.
3. collagen protein according to claim 1-PCL dentistry sthptic sponge is characterized in that its molecule of described collagen protein maintains the triple helix structure.
4. collagen protein according to claim 1-PCL dentistry sthptic sponge is characterized in that the ratio of collagen protein and PCL is counted 1:(4 ~ 20 by dry weight).
5. collagen protein according to claim 1-PCL dentistry sthptic sponge is characterized in that described auxiliary additive is any one or the two kinds of mixture in hemorrhage and the antiinflammatory antibacterial;
Described hemorrhage is any one or a few mixture in thrombin, YUNNAN BAIYAO, Radix Notoginseng, Herba Cirsii, Pseudobulbus Bletillae (Rhizoma Bletillae), the Pollen Typhae;
Described antiinflammatory antibacterial is any one or a few mixture in tea polyphenols, chitosan, benzylphenol, the tannin.
6. collagen protein according to claim 1-PCL dentistry sthptic sponge, the weight ratio that it is characterized in that auxiliary additive and collagen protein-PCL complex liquid is 1: (200~2000).
7. collagen protein according to claim 1-PCL dentistry sthptic sponge is characterized in that described collagen protein-PCL dentistry sthptic sponge can be used as the hemostatic material of exodontia and other postoperation of oral cavity.
CN2011101732910A 2011-06-25 2011-06-25 Collagen-polycaprolactone (PCL) dental hemostatic sponge and preparation method thereof Pending CN102228716A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103316330A (en) * 2012-06-28 2013-09-25 西藏贝珠雅药业有限公司 Formula and purposes of soft tissue trauma nursing material
CN107519524A (en) * 2017-09-21 2017-12-29 滨州医学院 A kind of polycaprolactone/collagen/quaternary ammonium salt electrospun composite fibers film and preparation method thereof
CN110192989A (en) * 2019-05-07 2019-09-03 深圳欧珈再生医学抗衰生物工程有限公司 For promoting skin progenitor cell and collagen mother cell regenerative compositions and preparation method
CN114588081A (en) * 2022-03-01 2022-06-07 湖南有美生物科技有限公司 Preparation method of tea polyphenol-pichia pastoris recombinant collagen sponge scaffold gel and application of sponge scaffold gel in repairing skin inflammation

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CN101695581A (en) * 2009-10-26 2010-04-21 西北大学 Method for preparing human-like collagen haemostatic sponge in scale
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103316330A (en) * 2012-06-28 2013-09-25 西藏贝珠雅药业有限公司 Formula and purposes of soft tissue trauma nursing material
CN103316330B (en) * 2012-06-28 2016-03-09 西藏贝珠雅药业有限公司 A kind of prescription of soft-tissue trauma nursing material and purposes
CN107519524A (en) * 2017-09-21 2017-12-29 滨州医学院 A kind of polycaprolactone/collagen/quaternary ammonium salt electrospun composite fibers film and preparation method thereof
CN110192989A (en) * 2019-05-07 2019-09-03 深圳欧珈再生医学抗衰生物工程有限公司 For promoting skin progenitor cell and collagen mother cell regenerative compositions and preparation method
CN110192989B (en) * 2019-05-07 2023-03-24 深圳欧珈再生医学抗衰生物工程有限公司 Composition for promoting regeneration of skin stem cells and collagen blasts and preparation method thereof
CN114588081A (en) * 2022-03-01 2022-06-07 湖南有美生物科技有限公司 Preparation method of tea polyphenol-pichia pastoris recombinant collagen sponge scaffold gel and application of sponge scaffold gel in repairing skin inflammation

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Application publication date: 20111102