Method of obtaining porous chitosan calcium phosphate-containing sponges for filling bone defects

FIELD: medicine.

SUBSTANCE: described is a method of obtaining a composite chitosan-based material, which contains aspartic or glutamine amino acids in a quantity from 2 to 5 wt %, as well as calcium phosphates with a ratio of Ca/P from 1.0 to 1.67. The method consists in barbotage through a suspension of calcium phosphates, obtained in situ in a solution of chitosan and aspartic or glutamic acid, with the following lyophilic drying of the foamed products. Porous matrices can be applied in dentistry, maxillofacial surgery, osteoplastic surgery as implants in the treatment of bone tissue defects.

EFFECT: obtained samples are characterised by a uniform porous structure with the simultaneous reduction of calcium phosphate dimensions to a nano-level with the reduction of the number of material obtaining operations.

2 dwg, 5 ex

 

The invention relates to composite materials for medicine, namely traumatology and Orthopaedics, maxillofacial surgery and surgical dentistry, and can be used for the manufacture of consolidated materials for filling bone defects.

Because the bone tissue is a composite material containing calcium phosphate (FC) and organic components (collagen, collagen biokompozitnyh produce and proteins), such a composition allows you to carry the mechanical loads, which are critical, for example, for ceramic bone implants. So promising is the use of composite materials containing both inorganic (FC), and organic components. In addition to collagen and gelatin as the organic component can be used chitosan. Chitosan is a biocompatible and biodegradable natural polymer, which allows its use in various fields of medicine, including for fast healing of different etymologies (Chitin and chitosan. Preparation, properties and application. Under the editorship of academician of the RAAS, K. G. Skryabin. Science. 2002. 365 p.). Especially widely used chitosan materials in the form of a plastic porous sponges. Due to the porosity of these materials are easily deformed to the desired RA�measure (bone defect) and after placing them in a compressed state in the bone defect straightened (due to the inverse deformation), filling the defect volume. Chitosan refers to polysaccharides, substances that promote the formation of bone tissue. However, chitosan sponges do not contain such important for the formation of bone elements, such as phosphorus and calcium. Therefore, when resorption such sponges in the bone defect formed mainly of cartilage (chondroitine). Calcium phosphates, such as dicalciumphosphate (DCPD), octacalcium phosphate (OCP), tricalcium phosphate (TCP), amortizatory calcium phosphate (ROS), precipitated hydroxyapatite (RSA), carbonate-bearing hydroxyapatite (KGA), other substituted forms of hydroxyapatite (HA), as a result of biodegradation in the human body under the action of biological fluids to form calcium ions and phosphate, contributing to the formation of bone tissue de novo.

In the prior art closest to the proposed technical solution and the achieved effect of the invention: RF patent №2376019 "Porous composite material based on chitosan and gelatin containing octacalcium to fill bone defects. Porous chitosan sponges were prepared as follows: powder of high molecular weight chitosan (molecular weight 450000-500000 g/mol) in 1 g of 33.3 wt.%) was dissolved in aqueous acetic acid. Then added with stirring 1 g of 33.3 wt.%) the HA granules (filler)with a grain size of 100-300 μm and 1 g of 33.3 wt.%) powder of ammonium carbonate. The result was plastic composite sponge with a porosity of 85%. The disadvantages of this invention are the necessity of using in the process of obtaining sponges acetic acid and ammonium carbonate, and also a large number of operations prior to the receipt of a porous chitosan sponges: synthesis of FC, their drying, disaggregation, molding and sintering the obtained FC materials.

In the patent of Russian Federation №2376019 C2 "Porous composite materials based on chitosan for filling of bone defects has been consolidated materials from porous composite matrix based on chitosan and FC (KMHFQ). Powder of high molecular weight chitosan (molecular weight 450000-500000 g/mol) in 1 g of 33.3 wt.%) was dissolved in acetic acid solution. Then under stirring was added 1 g of 33.3 wt.%) the HA granules (filler) with a grain size of 100-300 μm and 1 g of 33.3 wt.%) powder of ammonium carbonate. The resulting sponge was washed with ethanol and air dried to remove ethanol. The result was plastic composite sponge with a porosity of 85%. The disadvantage of the above invention are the use, for the expansion of ammonium carbonate and acetic acid, resulting in the formation of a byproduct, ammonium acetate, and the need for surgery washing from him.

The object of the present invention is the crea� biocompatible material, approximate in structure to natural bone tissue, while reducing the number of operations of receipt of materials.

The technical result of the present invention is to maintain the porosity of the material while reducing the size of the PC to nanorana (less than 100 nm) to reduce the number of operations of receipt of materials.

The technical result is achieved in that the porous chitosan sponge for filling bone defects containing FC, obtained by synthesis in situ FC in an aqueous solution containing chitosan and amino acid (glutamic or aspartic), taken in an amount of 2-5 wt.% when the temperature of the reaction mixture from 37 to 90°C, according to the invention, 30 minutes after the completion of the synthesis the reaction mixture was dried by bubbling air through it using compressor, after which the foam mixture is dried by freezing in freeze-dryer.

The essence of the invention consists in the synthesis of FC in situ in a solution containing chitosan, aspartic or glutamic acid, with the subsequent foaming of the slurry and drying it in freeze dryer. This method of obtaining porous chitosan matrices eliminates several operations - filtration step FC, drying, disaggregation (grinding in a planetary or ball mill) and a uniform distribution in the solution of chitosan and �asparaginovoi or glutamic acids. In addition, the proposed in the invention method for producing porous matrices allows to keep the size of the particles of calcium phosphates in chitosan matrix at the level of 30-70 nm, as in natural bone tissue. Nanorazmernoi particles FC in chitosan matrix is saved due to the absence of the drying process the received FC at which the agglomeration of particles and the formation of dense agglomerates and durable large aggregates.

During freeze-drying of foamed samples is the removal of water, in which water from a solid turns into a gas, bypassing the liquid state. This preserves the porous structure of the foamed sample.

Example 1

2 g of aspartic acid was dissolved in 100 ml of water, then in the resulting acid solution (pH 3.5 to 4.0) was dissolved 2 g of chitosan of high molecular weight (M. 300000 kDa) at 37°C. To the resulting solution was added 40 ml of a solution of calcium nitrate 1 mol/l, and then to the solution was added with stirring dropwise 40 ml of a solution of dibasic ammonium phosphate in a concentration of 1 mol/L. pH of the mixture at the end of synthesis at 5.5-6.0. 30 minutes after start of mix through suspensions were barbotirovany the air using a compressor. The foam mass was placed in the form, then produced the drying with the use�of freeze dryers. The main phase according to the XRD is DCPD, the diffraction patterns are also present in the band corresponding to aspartic acid and chitosan. The particle size of FC in chitosan matrix is in the range of 20-70 nm. The porosity of the material is in the range of 80-85%, the pores are interconnected.

Example 2

6 g of aspartic acid was dissolved in 100 ml of water, then in the resulting acid solution (pH 3.5 to 4.0) was dissolved 6 g of chitosan of high molecular weight (M. 300000 kDa) at a temperature of 60°C. Formed a very viscous suspension. When you add 60 ml of a solution of calcium nitrate solution with the slurry is not mixed, there was a formation of a homogeneous solution. After adding ammonium phosphate precipitate formed, which was unable to evenly distribute the suspension volume of chitosan. When you try to barbotirovany air through the reaction mixture the passage of air bubbles through the suspension proved to be impossible due to too high viscosity of the latter.

Example 3

1 g of aspartic acid was dissolved in 100 ml of water, then in the resulting acid solution (pH 2.5 to 3.0) was dissolved 1 g of chitosan of high molecular weight (M. 300000 kDa) at a temperature of 90°C. To the resulting solution was added 50 ml of a solution of calcium nitrate 1 mol/l, and then to the solution was added with stirring dropwise 30 ml of a solution of disodium FOS�ATA ammonium concentration of 1 mol/L. the pH of the mixture during the synthesis process was maintained in the range of 8.5-9.0 by the addition of ammonia solution. After 30 minutes of sedimentation, the suspension was foamed by bubbling air using a compressor. After foaming was too rapid settling of the foam, which is not given the opportunity to perform lyophilization preserving the structure of the foam. As a result of drying instead of a sponge formed powder due to low concentration of chitosan and consequently low viscosity suspension.

Example 4

5 g of glutamic acid was dissolved in 100 ml of water, then in the resulting acid solution (pH of 4.0) was dissolved 5 g of chitosan of high molecular weight (M. 300000 kDa). To the resulting solution was added 60 ml of a solution of calcium nitrate 1 mol/l, and then to the solution was added with stirring dropwise 40 ml of a solution of disodium phosphate ammonium concentration of 1 mol/L. pH of the mixture during the synthesis process was maintained at 7.0 by the addition of ammonia solution. 30 minutes after start of mix through suspensions were barbotirovany the air using a compressor. The foam mass was placed in the form, then produced the drying using freeze dryers. The main phase according to the XRD is AFK, are present in diffraction patterns of the bars corresponding to glutamic sour�e and chitosan. The particle size of FC in chitosan matrix is in the range of 20-70 nm. The porosity of the matrix was 70-80%, the pores are interconnected. In Fig. 1(a, b) presents the microstructure of the sample, confirming it.

Example 5

4 g of aspartic acid was dissolved in 100 ml of water, then in the resulting acid solution (pH 2.5 to 3.0) was dissolved 4 g of chitosan of high molecular weight (M. 300000 kDa) at a temperature of 90°C. To the resulting solution was added 50 ml of a solution of calcium nitrate 1 mol/l, and then to the solution was added with stirring dropwise 30 ml of a solution of disodium phosphate ammonium concentration of 1 mol/L. pH of the mixture during the synthesis process was maintained in the range of 8.5-9.0 by the addition of ammonia solution. After 30 minutes of sedimentation, the suspension was foamed by bubbling air using a compressor. After foaming the slurry was dried in freeze dryer. The main phase according to the XRD is RSA, which is confirmed by the strongly broadened peaks in diffraction patterns (Fig. 2), there are also bars corresponding to aspartic acid and chitosan. The particle size of FC in chitosan matrix is in the range of 60-90 nm. The porosity of the material is in the range of 80-85%, the pores are interconnected.

A method of producing a porous chitosan sponge containing calcium phosphates, for filling bone defects, ex�featuring the the in situ synthesis of calcium phosphates in aqueous solution containing chitosan and glutamic or aspartic acid, taken in an amount of 2-5 wt.%, carried out at a temperature of the reaction mixture from 37 to 90°C, 30 minutes after the completion of the synthesis the reaction mixture was dried by bubbling air through it using compressor, after which the foam mixture is dried by freezing in freeze-dryer.



 

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FIELD: chemistry.

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5 cl, 5 dwg

FIELD: physics.

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12 cl, 3 tbl, 21 ex

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3 cl, 3 ex

FIELD: medicine.

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2 cl, 1 dwg, 2 ex

FIELD: medicine.

SUBSTANCE: invention relates to medicine, namely to traumatology of the maxillofacial area, and can be applied for the treatment of mandibular fractures. For this purpose the reposition and fixation of bone fragments by means of osteosynthesis or dental splints are carried out. After the reposition and fixation of bone fragments, diluted with physiological solution or the local anaesthetic botulinum toxin A - Botox or B Myoblock is introduced once into the muscles, participating in the displacement of mandible fragments. The preparation is introduced with the distribution of the total volume and maximally allowed quantity of units by 20% in the area of muscle fixation to the bones and by 80% into the zone of the highest electric activity of the muscles, verified by the method of electromyography.

EFFECT: method provides an increased rigidity of fixation of the mandible bone fragments due to the reduction of a risk of displacement and mobility of the fragments, acceleration of consolidation processes.

2 ex

Siglec-15 antibody // 2539790

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to biotechnology and immunology. What is described is a pharmaceutical composition used for treating and/or preventing pathological bone metabolism and containing this antibody. The invention can be used in medicine.

EFFECT: antibody and its functional fragment specifically recognising human Siglec-15 and possessing the osteoclast inhibitory activity are described.

73 cl, 57 dwg, 4 tbl, 33 ex

FIELD: medicine.

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EFFECT: invention provides reducing a dose of the administered preparations and a rate of administration as compared to the systemic antibacterial therapy by an ability of the administered mixture to be accumulated in the inflammation centre, providing the therapeutic concentration with the total dose of the administered preparations reduced as compared to the systemic antibiotic therapy.

2 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: group of inventions refers to treating arthropathies, such as arthrosis and inflammatory loss of cartilage, tendon disorders and/or degenerative spine diseases. What is presented is a pharmaceutical composition for the above application, containing a corticosteroid and a cytokine antagonist - a natural or recombinant protein of interleukin IL-1Ra antagonist, particularly orthokine or anakinra, and optionally a growth factor; the composition is injectable into an injured nerve root, or into an injured intervertebral disk, or into their local context, or for intraarticular injection. There are presented: a kit comprising the pharmaceutical composition with the above cytokine antagonist and optionally the growth factor, and the pharmaceutical composition with the corticosteroid; using the above cytokine antagonist and optionally the growth factor for preparing the pharmaceutical composition to be used in combination therapy together with the corticosteroid for the above application; using the corticosteroid for preparing the pharmaceutical composition to be used in combination therapy with the above cytokine antagonist and optionally the growth factor for treating the above arthropathies, tendon disorders and/or degenerative spine diseases.

EFFECT: clinical success of treatment manifested by apparent joint detumescence, pain reduction by 60-100%, functional improvement of the joint, with the effect persisting 8 months later and more after the treatment.

39 cl, 1 tbl

FIELD: medicine.

SUBSTANCE: invention refers to medical and veterinary traumatology, surgery and concerns treating various bone injuries, particularly fractures and fissured fractures. That is ensured by fixing injured bone fragments with a plaster splint or a polymer bandage. An aqueous solution containing 1-hydroxyethylene diphosphonic aicd in an amount of 1.80-2.06 g/l, anhydrous calcium chloride in an amount of 1.44-2.22 g/l, gadolinium (III) nitrate hexahydrate in an amount of 0.30-0.40 g/l, dysprosium (III) chloride hexahydrate in an amount of 0.038-0.076 g/l is introduced into the fracture; pH of the solution is 7.3-7.8. Before administering into the fracture, the above agent is heated up to 30-100°C, kept at this temperature for 1-48 hours, and cooled to room temperature.

EFFECT: method provides reducing the osteoanagenesis time within the injury, including by providing the optimal thermodynamic crystalline maturing with low toxicity of the solution and its storage stability.

3 tbl, 35 ex

FIELD: medicine.

SUBSTANCE: what is applied is a stocking coating of an autogenous bone with a patient's platelet-rich plasma. Bone marrow aspirate from the patient's ilium and/or mesenchymal stromal cell autoculture prepared of the aspirate by culturing in vitro are injected under the coating layer into the autogenous bones. The autogenous bones are placed tightly in the bone defect to cover the defect area with adjacent soft tissues.

EFFECT: complete and effective synthesis of the bone tissue continuity by creating conditions of proliferative process isolation and osteoresorption process deceleration in the autogenous bone with no undesired immunological responses in the plasty area.

1 dwg, 1 ex

FIELD: medicine.

SUBSTANCE: invention represents an agent for treating a pulp inflammation differing by the fact that it contains Bezornil ointment and Dycal ivory paste in ratio 1:1 blended until smooth.

EFFECT: invention provides relieving oedema and pain on the day of doctor's appointment, accelerating the pulp tissue regeneration process, creating the reparative dentin within 30 days, and ensures the higher clinical effectiveness in the pulp inflammations.

2 ex, 1 tbl

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