CN-122005917-A - Lithium-doped silicon-based hydroxyapatite nanowire and preparation method and application thereof

CN122005917ACN 122005917 ACN122005917 ACN 122005917ACN-122005917-A

Abstract

The invention discloses a lithium-doped silicon-based hydroxyapatite nanowire, which has a chemical composition general formula of Ca x Li 20‑2x (P 1‑y Si y O 4 ) 6 (OH) 2 , wherein x is more than or equal to 0 and less than or equal to 9.09,0.05 and y is more than or equal to 0.12. The preparation method of the lithium-doped silicon-based hydroxyapatite nanowire comprises the steps of firstly preparing the lithium-doped calcium silicate nanowire by a hydrothermal method, and then preparing the lithium-doped silicon-based hydroxyapatite nanowire by the hydrothermal method. The invention combines the bionic osteogenesis induction characteristic of the nano-level hydroxyapatite material with the regulation of bone metabolic homeostasis and immune response of lithium and silicon elements, adjusts the preparation conditions and chemical components of the material to obtain the lithium-doped silicon-based hydroxyapatite nanowire doped with the lithium elements in proper proportion, and provides a new thought for tissue engineering immunotherapy of inflammatory periodontal bone defects by regulating and controlling periodontal tissue immune microenvironment and maintaining bone metabolic balance.

Inventors

XIA LUNGUO
FANG BING
ZHU ZHIYU
LI RUOMEI
MEI PENG
ZHU CHENG
JIN YU

Assignees

上海交通大学医学院附属第九人民医院

Dates

Publication Date: 20260512
Application Date: 20241108

Claims (11)

1. The lithium-doped silicon-based hydroxyapatite nanowire is characterized in that the chemical composition general formula of the lithium-doped silicon-based hydroxyapatite nanowire is Ca x Li 20-2x (P 1-y Si y O 4 ) 6 (OH) 2 , wherein x is more than 0 and less than 10, and y is more than or equal to 0.05 and less than or equal to 0.12; The morphology of the lithium-doped silicon-based hydroxyapatite nanowire is nanowire.
2. The lithium-doped silicon-based hydroxyapatite nanowire according to claim 1, wherein the length of the lithium-doped silicon-based hydroxyapatite nanowire is 70-130 nanometers and the diameter is 5-25 nanometers.
3. A method for preparing the lithium-doped silicon-based hydroxyapatite nanowire according to claim 1, wherein the preparation method comprises the following steps: s1, respectively dissolving soluble calcium salt, soluble lithium salt and soluble silicate in double distilled water at room temperature, and fully stirring and dissolving to obtain solutions 1-3 respectively; S2, mixing the solutions 1-3 obtained in the step S1, and fully stirring to obtain a solution 4; S3, carrying out a high-temperature hydrothermal reaction on the solution 4 obtained in the step S2 to obtain a solid-liquid mixture 1; S4, washing and suction filtering the solid-liquid mixture 1 obtained in the step S3 by using a vacuum suction filtering device, sufficiently drying, grinding, and sieving with a 400-mesh sieve to obtain the lithium-doped calcium silicate nanowire; s5, dissolving soluble phosphate in double distilled water at room temperature, and fully stirring to obtain a solution 5; S6, mixing the lithium-doped calcium silicate nanowire obtained in the step S4 and the solution 5 obtained in the step S5, and fully stirring to obtain a solid-liquid mixture 2; S7, carrying out a hydrothermal reaction on the solid-liquid mixture 2 obtained in the step S6 to obtain a solid-liquid mixture 3; And S8, washing and suction filtering the solid-liquid mixture 3 obtained in the step S7 by using a vacuum suction filtering device, sufficiently drying, grinding, and sieving with a 400-mesh sieve to obtain the lithium-doped silicon-based hydroxyapatite nanowire.
4. The process according to claim 3, wherein in step S1, The soluble calcium salt is selected from one or more of calcium nitrate tetrahydrate and calcium chloride dihydrate, and/or, The soluble lithium salt is selected from one or more of lithium chloride monohydrate and lithium nitrate, and/or, The soluble silicate is selected from one or more of sodium silicate nonahydrate and potassium silicate, and/or, In the mixed solution of the soluble calcium salt and the soluble lithium salt, the element mole ratio Li (Li+Ca) is in the range of (0,0.2), and/or, The element mole ratio of the soluble calcium salt, the soluble lithium salt and the soluble silicate is (Ca+Li): si is in the range of (0.8,1.2), and/or, The stirring speed is 100-300 rpm, and/or, The stirring time is 1.5-4 hours.
5. The process according to claim 3, wherein in step S2, The stirring speed is 100-300 rpm, and/or, The stirring time is 1.5-4 hours.
6. The process according to claim 3, wherein in step S3, The temperature of the high-temperature hydrothermal reaction is 180-200 ℃, and/or, The time of the high-temperature hydrothermal reaction is 24-72 hours.
7. The process according to claim 3, wherein in step S5, The soluble phosphate is selected from one or more of sodium phosphate dodecahydrate and potassium phosphate monohydrate, and/or, The stirring speed is 100-300 rpm, and/or, The stirring time is 1.5-4 hours.
8. The process according to claim 3, wherein, in said step S6, The mass ratio of the soluble phosphate to the lithium-doped calcium silicate nanowire is (5-8): 1, and/or, The stirring speed is 100-300 rpm, and/or, The stirring time is 1.5-4 hours.
9. The process according to claim 3, wherein, in said step S7, The temperature of the high-temperature hydrothermal reaction is 120-180 ℃ and/or, The time of the high-temperature hydrothermal reaction is 24-72 hours.
10. The lithium-doped silicon-based hydroxyapatite nanowire prepared by the preparation method according to any one of claims 3 to 9, wherein the lithium-doped silicon-based hydroxyapatite nanowire can regulate the periodontal tissue immune microenvironment and maintain the bone metabolism balance.
11. Use of a lithium doped silicon based hydroxyapatite nanowire according to claim 1 or 2, or a method of preparation according to any of claims 3 to 9, a lithium doped silicon based hydroxyapatite nanowire according to claim 10 for the preparation of an inflammatory periodontal bone defect repair material.

Description

Lithium-doped silicon-based hydroxyapatite nanowire and preparation method and application thereof Technical Field The invention belongs to the technical field of biological materials, and relates to a lithium-doped silicon-based hydroxyapatite nanowire, a preparation method thereof and application thereof in preparation of inflammatory bone defect repair materials. Background Periodontitis is a common oral disease affecting more than about half of the population worldwide. In the fourth national oral epidemiological investigation report, the incidence of moderate-severe periodontitis in chinese adults was 62.4%, and the periodontal health rate was only 9.1%. Periodontitis is an inflammatory disease in which plaque biofilm is the initiating factor and the secondary local immune response disorder causes damage to periodontal soft and hard supporting tissues. The local immune response of periodontitis involves the participation and regulation of various immune cells, and T lymphocyte subpopulations have specific functions and roles in pathophysiological processes. Wherein, gamma delta T lymphocytes are specifically enriched in human mucous membrane epithelium, have bidirectional regulation and control in periodontal tissues, and secreted IL-17 and the like can enhance the activity of osteoclasts and promote the damage of periodontal tissues. Periodontitis and its accompanying lesions can cause alveolar bone absorption, thereby resulting in loosening or even loss of teeth, and the like, which have a great influence on oral health, function, beauty and patient life quality. Traditional methods for the use of bone grafting for inflammatory periodontal bone defects include autogenous bone grafting, allogeneic bone grafting, xenogeneic bone grafting, and the like. However, these methods all suffer from problems of scarcity, high price, large rejection reaction, and the like. Therefore, tissue engineering regeneration and repair become a hot spot in recent years. The inorganic material has the advantages of high hardness, high elastic modulus, good biocompatibility and the like, and is suitable for repairing bone defects. Therefore, how to utilize biological materials to regenerate and repair inflammatory bone defects aiming at the immunopathological characteristics of periodontitis is one of the problems to be solved in the technical field. Hydroxyapatite is an inorganic material widely applied to bone repair as an inorganic component in hard tissues of vertebrates. However, the single-component hydroxyapatite has limited osteoinductive performance, and is often modified by the method comprising special morphology structure regulation, chemical component modification and the like. The nano-level hydroxyapatite has unique properties such as surface effect, small-size effect, quantum effect and the like, can promote cell spreading adhesion, protein adsorption, induce osteogenic differentiation, accelerate osseointegration and bone reconstruction, and promote bone regeneration. The lithium salt is a classical mental disease drug, and researches show that the lithium salt also has the effects of maintaining bone metabolic homeostasis, promoting bone repair and regeneration, regulating lymphocyte immune response and the like. The silicon-substituted biomaterial exhibits excellent angiogenic and osteogenic properties while inhibiting osteoclast regeneration, and plays a regulatory role in innate immunity. Therefore, the novel biological material of the silicon-based hydroxyapatite with the combination of the lithium element and the silicon element provides potential possibility for the regeneration and repair of inflammatory bone defects aiming at the immunopathology characteristics of periodontitis. At present, no application example of the lithium-doped silicon-based hydroxyapatite nanowire prepared by a hydrothermal method for regulating and controlling periodontal tissue immune microenvironment and inflammatory periodontal bone defect repair exists. Disclosure of Invention In order to solve the defects in the prior art, the invention aims to provide a lithium-doped silicon-based hydroxyapatite nanowire and a preparation method thereof, and the lithium-doped silicon-based hydroxyapatite nanowire is applied to the regulation and control of periodontal tissue immune microenvironment and the regeneration repair treatment of inflammatory periodontal bone defect. Based on the design of full-period regulation of the immunopathology process of periodontitis, the invention combines the immune regulation effect of lithium and silicon elements and the bone differentiation promoting effect of the hydroxyapatite nano material, and the lithium element is doped into the nano-level silicon-based hydroxyapatite material, so that the lithium-based hydroxyapatite nano material has the potential of full-period regulation of the immune homeostasis of periodontal soft and hard tissues and promotion of regeneration and repair of inflammat