CN112755241A - Dimethyloxalyl glycine-nano silicate fiber membrane and preparation method thereof - Google Patents
Dimethyloxalyl glycine-nano silicate fiber membrane and preparation method thereof Download PDFInfo
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- CN112755241A CN112755241A CN202011617795.2A CN202011617795A CN112755241A CN 112755241 A CN112755241 A CN 112755241A CN 202011617795 A CN202011617795 A CN 202011617795A CN 112755241 A CN112755241 A CN 112755241A
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- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
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Abstract
The invention belongs to the technical field of materials for promoting tissue regeneration, and particularly relates to a dimethyloxalyl glycine-nano silicate fiber membrane and a preparation method thereof. The invention utilizes high-voltage electrostatic spinning technology to produce the nanofiber membrane, PLGA is dissolved in hexafluoroisopropanol, DMOG and nSi are added and then dissolved in hexafluoroisopropanol solution of PLGA for electrostatic spinning, the position of the nanofiber membrane formation is controlled by adjusting an electric field, the nanofiber membrane can be completely and continuously formed on the surface of a collector, and the obtained nanofiber membrane can be used as a coupled double-release structure for coordinating and enhancing osteogenesis-angiogenesis. Compared with bioactive protein substances, the dimethyloxalylglycine-nano silicate fiber membrane is more stable, more economical and more suitable for clinical translation to realize optimal periodontal regeneration.
Description
Technical Field
The invention belongs to the technical field of materials for promoting tissue regeneration, and particularly relates to a dimethyloxalyl glycine-nano silicate fiber membrane and a preparation method thereof.
Background
Periodontal disease is a chronic inflammatory disease, caused by cross infection of a series of periodontal pathogens, which causes inflammation of gums, gradually induces damage to periodontal soft tissue and loss of bone tissue, thereby affecting the integrity of supporting tissues of teeth, usually causing inflammation of gingival tissue, irreversible adhesion loss, alveolar bone resorption and tooth mobility, and finally may cause loss of periodontal tissue or tooth loss, thereby endangering human oral health. Currently, there are several achievements in the clinical adaptation of periodontal regenerative medicine focusing on cell therapy, signaling molecules and techniques for inducing bone regeneration. Topical application of bioactive substances is an effective method of promoting periodontal tissue regeneration, stimulating new bone formation, inducing bone regeneration, and repairing defective alveolar bone, most commonly growth factors or chemokines. However, these biologically active proteins have several disadvantages, such as short half-life, poor protein stability, high dosage requirements, undesirable side effects and high cost, which limit their clinical use.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a dimethyloxalyl glycine-nano silicate fiber membrane, aiming at solving the technical problems that bioactive protein for treating periodontal diseases in the prior art has the defects of short half-life, poor protein stability, high dosage requirement, adverse side effect and high cost, thereby limiting clinical application, so that the preparation method can be used for preparing a nano fiber membrane material for promoting periodontal tissue regeneration, can well repair alveolar bone defects, and has good application prospect in the field of periodontal repair.
The invention provides a preparation method of a dimethyloxalyl glycine-nano silicate fiber membrane, which has the following specific technical scheme:
the preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane comprises the following steps:
s1, dissolving polylactide-glycolide into hexafluoroisopropanol, and stirring for dissolving to obtain a polymer solution;
s2, adding dimethyloxalglycine and nano silicate into the polymer solution obtained in the step S1, performing ultrasonic treatment, and stirring to obtain an electrospinning solution;
s3, the electrospinning solution obtained in the step S2 is filled into a syringe for electrostatic spinning, so that nanofibers are obtained and dried, and the dimethyloxalyl glycine-nano silicate fiber membrane is obtained.
In certain embodiments, in step S1, the polylactide-glycolide has a molecular weight of 9 ten thousand, and the molar ratio of lactide to glycolide in the polylactide-glycolide is 3: 1; the concentration of the polylactide-glycolide in the polymer solution is 20-25W/V%.
In certain embodiments, in step S1, the temperature of the stirring is 17 to 25 ℃, and the time of the stirring is 10 to 20 hours. The specific value of the stirring time of the solution is determined according to the actual solution condition, and the solution is ensured to be uniform and stable.
In certain embodiments, in step S2, the mass ratio of dimethyloxalylglycine, nanosilicate, and polylactide-glycolide in the polymer solution is 1:5: 100.
in certain embodiments, in step S2, the sonication time is 10 to 30 minutes and the stirring time is 2 to 5 hours.
In some embodiments, in step S3, in the electrostatic spinning, the spinning voltage is 10-15KV, the advancing speed is 2-5ml/h, and the receiving distance is 15-20 cm. In order to obtain a stable flow of the polymer solution during electrospinning, the spinning voltage and the advancing speed can be appropriately adjusted. The viscosity of the spinning solution with different proportions is different, so that the viscosity of the electrospinning solution can be adjusted according to the actual viscosity of the electrospinning solution.
In certain embodiments, in step S3, the electrospinning temperature is 18 to 25 ℃ and the relative humidity is 50 to 60%; the drying temperature is 17-25 ℃, and the drying time is 5-15 hours.
The invention also provides a technical scheme of the dimethyloxalyl glycine-nano silicate fiber membrane, and the dimethyloxalyl glycine-nano silicate fiber membrane prepared by the method.
Dimethyloxalylglycine (DMOG) is a small molecule permeable to cells and is a pharmacological inhibitor of Prolyl Hydroxylase (PHD). DMOG, as a powerful small angiogenic molecule, is very beneficial for tissue regeneration. For example, a fiber membrane loaded with DMOG can significantly accelerate healing of diabetic wounds and improve angiogenesis. Various DMOG drug-loaded scaffolds have also been shown to promote bone healing by promoting angiogenesis. In addition, PHD inhibition can reduce the inflammatory response and protect against various inflammatory diseases, while DMOG can reduce Lipopolysaccharide (LPS) -induced production of inflammatory mediators in human gingival fibroblasts. Thus, DMOG may serve as a promising bioactive molecule for periodontal tissue regeneration. The nano silicate is composed of bioactive silicate nano sheets and is a synthetic two-dimensional disc-shaped nano material with the diameter of 20-50nm and the height of 1-2 nm. In aqueous solution, nSi can be broken down into non-toxic ionic products that can trigger cellular reactions associated with tissue regeneration. Silicon is an essential element in the growth and metabolic processes of skeletal tissue and can promote the formation and calcification of new skeletal tissue. The invention utilizes high-voltage electrostatic spinning technology to produce the nanofiber membrane, PLGA is dissolved in hexafluoroisopropanol, DMOG and nSi are added and then dissolved in hexafluoroisopropanol solution of PLGA for electrostatic spinning, the position of the nanofiber membrane formation is controlled by adjusting an electric field, the nanofiber membrane can be completely and continuously formed on the surface of a collector, and the obtained nanofiber membrane can be used as a coupled double-release structure for coordinating and enhancing osteogenesis-angiogenesis. Compared with bioactive protein substances, the dimethyloxalylglycine-nano silicate fiber membrane is more stable, more economical and more suitable for clinical translation to realize optimal periodontal regeneration.
Drawings
Fig. 1 is a flow chart of a method for preparing a dimethyloxalylglycine-nano silicate fiber membrane provided by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings 1 in conjunction with specific embodiments.
Example 1
The preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane provided by the embodiment has the following specific technical scheme:
the preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane comprises the following steps:
(1) preparation of Polymer solution
First, 100g of polylactide-glycolide (PLGA) was added to hexafluoroisopropanol, and dissolved with stirring at room temperature (17-25 ℃ C.) for 10 hours to prepare a 20% (W/V) polymer solution.
(2) Preparation of electrospinning solution
Then 1g Dimethyloxalylglycine (DMOG) and 5g nano silicate (nSi) were added to the above polymer solution, sonicated in a sonicator for 15 minutes, mixed and stirred for 2 hours to obtain a homogeneous solution (electrospinning solution).
(3) Preparation of dimethyloxalyl glycine-nano silicate fiber membrane
And (3) filling the electrospinning solution into a 5ml syringe with a metal needle, wherein the distance from the needle point to a receiver covered with an aluminum foil is 18cm, the spinning voltage is 12KV, and the propelling speed is 3ml/h, so that the nanofiber membrane is obtained. The temperature in the spinning process is 18-25 ℃, and the relative humidity is 50-60%. After spinning was complete, the nanofiber membrane was separated from the collector and dried at room temperature (17-25 ℃) for 5 h.
This example also provides a dimethyloxalylglycine-nanosilicate fibrous membrane prepared according to the above method.
Example 2
The preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane provided by the embodiment has the following specific technical scheme:
the preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane comprises the following steps:
(1) preparation of Polymer solution
First, 200g of polylactide-glycolide (PLGA) was added to hexafluoroisopropanol, and dissolved at room temperature (17-25 ℃ C.) with stirring for 15 hours to prepare a 25% (W/V) polymer solution.
(2) Preparation of electrospinning solution
2g of Dimethyloxalylglycine (DMOG) and 10g of nano silicate (nSi) were added to the above polymer solution, and subjected to ultrasonic treatment in an ultrasonic instrument for 30 minutes, followed by mixing and stirring for 5 hours to obtain a uniform solution (electrospinning solution).
(3) Preparation of dimethyloxalyl glycine-nano silicate fiber membrane
And (3) filling the electrospinning solution into a 5ml syringe with a metal needle, wherein the distance between the needle point and a receiver covered with an aluminum foil is 20cm, the spinning voltage is 15KV, and the propelling speed is 5ml/h, so that the nanofiber membrane is obtained. The temperature in the spinning process is 18-25 ℃, and the relative humidity is 50-60%. After spinning was complete, the nanofiber membrane was separated from the collector and dried at room temperature (17-25 ℃) for 10 h.
This example also provides a dimethyloxalylglycine-nanosilicate fibrous membrane prepared according to the above method.
Example 3
The preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane provided by the embodiment has the following specific technical scheme:
the preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane comprises the following steps:
(1) preparation of Polymer solution
150g of polylactide-glycolide (PLGA) was first added to hexafluoroisopropanol and dissolved with stirring at room temperature (17-25 ℃ C.) for 20 hours to prepare a 22% (W/V) polymer solution.
(2) Preparation of electrospinning solution
Then, 1.5g of Dimethyloxalylglycine (DMOG) and 7.5g of nano silicate (nSi) were added to the above polymer solution, and subjected to ultrasonic treatment in an ultrasonic instrument for 10 minutes, followed by mixing and stirring for 3 hours to obtain a uniform solution (electrospinning solution).
(3) Preparation of dimethyloxalyl glycine-nano silicate fiber membrane
And (3) filling the electrospinning solution into a 5ml syringe with a metal needle, wherein the distance from the needle point to a receiver covered with an aluminum foil is 15cm, the spinning voltage is 10KV, and the propelling speed is 2ml/h, so that the nanofiber membrane is obtained. The temperature in the spinning process is 18-25 ℃, and the relative humidity is 50-60%. After spinning was complete, the nanofiber membrane was separated from the collector and dried at room temperature (17-25 ℃) for 15 h.
This example also provides a dimethyloxalylglycine-nanosilicate fibrous membrane prepared according to the above method.
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the invention, and the present invention is not limited to the above examples, and those skilled in the art should also be able to make various changes, modifications, additions or substitutions within the spirit and scope of the present invention.
Claims (8)
1. The preparation method of the dimethyloxalyl glycine-nano silicate fiber membrane is characterized by comprising the following steps of:
s1, dissolving polylactide-glycolide into hexafluoroisopropanol, and stirring for dissolving to obtain a polymer solution;
s2, adding dimethyloxalglycine and nano silicate into the polymer solution obtained in the step S1, performing ultrasonic treatment, and stirring to obtain an electrospinning solution;
s3, the electrospinning solution obtained in the step S2 is filled into a syringe for electrostatic spinning, so that nanofibers are obtained and dried, and the dimethyloxalyl glycine-nano silicate fiber membrane is obtained.
2. The method for preparing dimethyloxalylglycine-nanosilicate fiber membrane of claim 1, wherein, in step S1, the molecular weight of the polylactide-glycolide is 9 ten thousand, and the molar ratio of lactide to glycolide in the polylactide-glycolide is 3: 1; the concentration of the polylactide-glycolide in the polymer solution is 20-25W/V%.
3. The method for preparing dimethyloxalylglycine-nanosilicate fiber membrane according to claim 1, wherein the stirring temperature is 17 to 25 ℃ and the stirring time is 10 to 20 hours in step S1.
4. The method for producing dimethyloxalylglycine-nanosilicate fiber membrane according to claim 1, wherein in step S2, the mass ratio of dimethyloxalylglycine, nanosilicate, and polylactide-glycolide in the polymer solution is 1:5: 100.
5. The method for preparing dimethyloxalylglycine-nanosilicate fiber membrane according to claim 1, wherein in step S2, the time of the ultrasonic treatment is 10 to 30 minutes, and the time of the stirring is 2 to 5 hours.
6. The method for preparing dimethyloxalylglycine-nanosilicate fiber membrane according to claim 1, wherein in step S3, the electrospinning voltage is 10 to 15KV, the advancing speed is 2 to 5ml/h, and the receiving distance is 15 to 20 cm.
7. The method for preparing dimethyloxalylglycine-nanosilicate fiber membrane according to claim 1, wherein in step S3, the temperature of the electrospinning is 18 to 25 ℃, and the relative humidity is 50 to 60%; the drying temperature is 17-25 ℃, and the drying time is 5-15 hours.
8. Dimethoxalylglycine-nanosilicate fibrous membrane, characterized in that a Dimethoxalylglycine-nanosilicate fibrous membrane prepared according to the method of any of claims 1-7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114272443A (en) * | 2021-12-10 | 2022-04-05 | 中国科学院上海硅酸盐研究所 | Preparation method and application of zinc silicate nanoparticle composite fiber scaffold |
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| CN103603138A (en) * | 2013-11-15 | 2014-02-26 | 无锡中科光远生物材料有限公司 | Preparation method of PLGA fibrous coat used for corneal tissue transplant |
| CN107551311A (en) * | 2017-08-25 | 2018-01-09 | 上海师范大学 | A kind of porous composite electrospun tunica fibrosa of orientation of controlled drug release and its preparation method and application |
| CN108411495A (en) * | 2018-02-07 | 2018-08-17 | 清华大学 | Self-bone grafting film and preparation method thereof |
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- 2020-12-31 CN CN202011617795.2A patent/CN112755241A/en active Pending
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|---|---|---|---|---|
| CN103603138A (en) * | 2013-11-15 | 2014-02-26 | 无锡中科光远生物材料有限公司 | Preparation method of PLGA fibrous coat used for corneal tissue transplant |
| CN107551311A (en) * | 2017-08-25 | 2018-01-09 | 上海师范大学 | A kind of porous composite electrospun tunica fibrosa of orientation of controlled drug release and its preparation method and application |
| CN108411495A (en) * | 2018-02-07 | 2018-08-17 | 清华大学 | Self-bone grafting film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| LINGLING SHANG等: "Dimethyloxallyl glycine/nanosilicates-loaded osteogenic/angiogenic difunctional fibrous structure for functional periodontal tissue regeneration", 《BIOACTIVE MATERIALS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114272443A (en) * | 2021-12-10 | 2022-04-05 | 中国科学院上海硅酸盐研究所 | Preparation method and application of zinc silicate nanoparticle composite fiber scaffold |
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