WO2004094335A1 - Calcium phosphate cement, use and preparation thereof - Google Patents
Calcium phosphate cement, use and preparation thereof Download PDFInfo
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- WO2004094335A1 WO2004094335A1 PCT/US2004/011637 US2004011637W WO2004094335A1 WO 2004094335 A1 WO2004094335 A1 WO 2004094335A1 US 2004011637 W US2004011637 W US 2004011637W WO 2004094335 A1 WO2004094335 A1 WO 2004094335A1
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- ttcp
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- whiskers
- paste
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/02—Surgical adhesives or cements; Adhesives for colostomy devices containing inorganic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/02—Phosphate cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/02—Phosphate cements
- C04B12/025—Phosphates of ammonium or of the alkali or alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
- C04B28/344—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
- C04B28/346—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition as a mixture of free acid and one or more phosphates
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/14—Phosphates
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00034—Physico-chemical characteristics of the mixtures
- C04B2111/00086—Mixtures with prolonged pot-life
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00034—Physico-chemical characteristics of the mixtures
- C04B2111/00206—Compositions defined by their elemental analysis
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/0025—Compositions or ingredients of the compositions characterised by the crystal structure
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00836—Uses not provided for elsewhere in C04B2111/00 for medical or dental applications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
- Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
Definitions
- the present invention relates generally to a calcium phosphate cement, and particularly to a fast-setting calcium phosphate cement, for use in dental and bone prosthesis.
- CPC calcium phosphate cement
- the prior art calcium phosphate cements suffer one or more drawbacks as follows: 1) requiring additives with a relatively poor bioactivity; 2) a complicated preparation process; 3) an undesired setting time or working time for the CPC that is difficult to adjust; 4) being incapable of setting to a desired shape in water, blood or body fluid; and 5) having poor initial strength after setting of the CPC.
- the present invention is based on the discovery that monophasic particles of tetracalcium phosphate (TTCP) having whiskers or fine crystals on surfaces of the particles can be prepared and used to make a calcium phosphate cement suitable for preparation of bone and tooth prosthesis.
- TTCP tetracalcium phosphate
- the invention provides calcium phosphate cement particles comprising monophasic tetracalcium phosphate (TTCP) particles, wherein said TTCP particles on their surfaces have whiskers or fine crystals with a width ranging from 2 to 500 nm and a length ranging from 5 to 5000 nm.
- TTCP monophasic tetracalcium phosphate
- the invention provides methods for preparing a paste for use in treating a defect in a bone or a tooth in a patient by introducing said paste into a bone defect or bone cavity of said patient or shaping said paste and implanting the resulting shaped paste into a bone defect or a bone cavity of said patient, said method comprising mixing invention TTCP particles and a hardening aqueous solution sufficient to form a paste.
- the invention provides methods for preparing TTCP particles comprising mixing a powder or small pieces of invention TTCP particles with a wetting agent, and controlling growth of whiskers or fine crystals of TTCP on surfaces of said TTCP powder or small pieces of TTCP by a controlling treatment, to provide whiskers or fine crystals of TTCP having a width ranging from 1 nm to 100 nm and a length ranging from 1 nm to 5000 nm.
- the present invention provides a calcium phosphate cement comprising monophasic TTCP particles having a diameter of 0.05 to 100 microns, wherein said TTCP particles on their surfaces have whiskers or fine crystals having a width ranging from 2 to 500 nm and a length ranging from 5 to 5000 nm, for example a width ranging from 2 to 100 nm and a length ranging from 5 to 1000 nm, or a width ranging from 2 nm to about 200 nm and a length ranging from 10 nm to about 2000 nm.
- a suitable process for preparing the calcium phosphate cement of the present invention comprises mixing a TTCP powder or small pieces of monophasic TTCP with a wetting agent, and controlling growth of whiskers or fine crystals on surfaces of said TTCP powder or small pieces of TTCP by an controlling treatment.
- the shape of the monophasic small pieces of TTCP or grains of TTCP powder are not limited, and can include spherical or irregular shapes; and the crystal structure thereof can be single crystal, polycrystal, mixed crystals, semi-crystal, or amorphous.
- Suitable wetting agents used to wet the powder or small pieces of TTCP include any aqueous solution comprising alkaline ions (for example, sodium(Na) or potassium(K) ions); alkaline earth ions (for example, magnesium(Mg) or calcium(Ca)
- the wetting agent used is a diluted aqueous solution containing phosphoric acid or phosphate.
- the amount of the wetting agent mixed with the monophasic TTCP powder or small pieces should be enough to substantially wet all the TTCP powder or small pieces of TTCP.
- the controlling treatment is the organic solvent treatment, where a water miscible organic solvent is added to the mixture of said wetting agent and the TTCP powder or small pieces of TTCP to form a paste for a subsequent processing step.
- a dilute aqueous solution containing more than 20 ppm of phosphoric acid or phosphate, more preferably more than 50 ppm, and most preferably more than 100 ppm of phosphoric acid or phosphate can be mixed with the monophasic TTCP particles or powder prior to the controlling treatment.
- the controlling treatment is selected from a vacuuming treatment, an organic solvent treatment, a microwave treatment, a heating treatment, or any other treatments that can control growth of whiskers or fine crystals on surfaces of monophasic TTCP powder or small pieces. Due to its simplicity and effectiveness, the most frequently used controlling treatment is heating to about 50 °C for 1 day. [0013]
- the process for preparing the calcium phosphate cement can further comprise grinding the resulting product from the controlling treatment to form TTCP particles having a diameter of 0.05 to 100 microns, wherein said whiskers or fine crystals of TTCP have a width ranging from 1 to 100 nm and a length ranging from 1 to 1000 nm.
- the process for preparing the calcium phosphate cement of the present invention comprises soaking said TTCP powder or said small pieces of TTCP with a diluted aqueous solution containing more than 100 ppm of phosphoric acid or phosphate, and carrying out (a) a heating treatment comprising drying the resulting soaked TTCP powder or soaked small pieces of TTCP at a temperature in the range from about 50°C to about ; (b) a vacuuming treatment comprising drying the resulting soaked TTCP powder or soaked small pieces of TTCP under vacuum; or (c) a microwave treatment comprising drying the resulting soaked-TTCP powder or soaked small pieces of TTCP by microwave heating. More preferably, the resulting soaked TTCP powder or soaked small pieces of TTCP are well mixed to form a uniform mixture prior to being subjected to treatment (a), (b) or (c).
- the process for preparing the calcium phosphate cement of the present invention comprises mixing the TTCP powder or the small pieces of TTCP with the diluted aqueous solution containing more than 100 ppm of phosphoric acid or phosphate, and carrying out the organic solvent treatment comprising mixing the mixture of the wetting agent and the TTCP powder or small pieces of TTCP with a water miscible organic solvent, and drying the resulting mixture under vacuum.
- the organic solvent treatment is carried out while stirring, and more preferably, the mixture of the diluted aqueous solution containing more than 100 ppm of phosphoric acid or phosphate and the TTCP powder or small pieces of TTCP is well mixed prior to being subjected to the organic solvent treatment.
- the TTCP particles of the calcium phosphate cement of the present invention have a diameter of 0.2 to 80 microns, and more preferably 0.5 to 50 microns.
- the " width" of a whisker means an average value of lateral cross- sectional diameters of the whisker
- the "width" of a fine crystal means an average value of the first 30% of the diameters of the fine crystal, which are shorter than the other 70% thereof.
- the "length" of a fine crystal means an average value of the last 30% of the diameters of the fine crystal, which are longer than the other 70% thereof.
- the whiskers or fine crystals of TTCP have a width ranging from 2 to 70 nm and a length ranging from 5 to 800 nm, and more preferably a length ranging from 10 to 700 nm.
- the TTCP particles have a molar ratio of calcium to phosphate ranging from 0.5 to 2.5, more preferably 0.8 to 2.3, and most preferably 1.0 to 2.2.
- the calcium phosphate cement of the present invention is biocompatible and a paste made therefrom is non-dispersive in water.
- the paste has a working time from several minutes to hours and a setting time from a few minutes to hours. Consequently, the calcium phosphate cement of the present invention is extremely suitable for use as an implant or filling material in dental or bone prostheses, where the paste must contact water, blood or body fluid when implanted.
- the paste made from the calcium phosphate cement of the invention is suitable for direct injection into a bone defect or cavity as an implant or filling material.
- the present invention also discloses a method of treating a defect in bone or a tooth in a patient, by mixing the calcium phosphate cement of the present invention with a hardening -promoter-containing aqueous solution to form a paste, and a) injecting the paste into a bone defect or cavity of said patient or b) shaping the paste and implanting the resulting shaped paste into a bone defect or cavity of the patient.
- the calcium phosphate cement may further comprise an agent that promotes bone growth, such as a growth factor, a bone morphology protein or a pharmaceutical carrier, or the hardening-promoter-containing aqueous solution can further comprises such an agent, for example, a growth factor, a bone morphology protein or a pharmaceutical carrier.
- an agent that promotes bone growth such as a growth factor, a bone morphology protein or a pharmaceutical carrier
- the hardening-promoter-containing aqueous solution can further comprises such an agent, for example, a growth factor, a bone morphology protein or a pharmaceutical carrier.
- the hardening-promoter-containing aqueous solution can further comprise any known compound or composition that promotes the solidification of calcium phosphate, for example phosphates, calcium salts, and fluorides.
- the hardening- promoter-containing aqueous solution may be an aqueous solution comprising phosphate ions, calcium ions, fluorine ions, or phosphate ions together with additional fluorine ions as a hardening promoter.
- the amount of the hardening promoter in the hardening-promoter-containing aqueous solution has no special limitation, but preferably the concentration of the hardening promoter therein ranges from 0.1 M to 8 M, and more preferably from 1 M to 6 M.
- the mixing ratio of the calcium phosphate cement of the present invention and the hardening-promoter-containing aqueous solution is not restricted to any particular ranges; however, the amount of said hardening-promoter-containing aqueous solution in the mixture should be sufficient to provide substantial wetting of the calcium phosphate cement of the present invention. It should be noted that more water can be supplied in- situ from saliva or body fluid when the paste is injected or implanted into the bone defect or cavity. Furthermore, the amount of the hardening promoter in the hardening-promoter- containing aqueous solution should be adjusted to a higher level when a lesser amount of said hardening-promoter-containing aqueous solution is used in the mixture.
- a "subject" as the term is used herein is any mammal, including zoo, farm and domestic animals and humans.
- an "effective amount" of the injectable calcium-phosphate-based bone substitute as the term is used herein is an amount effective to accomplish fusion of vertebrae adjacent to the interbody site in the subject.
- Setting time is the time after which a 1 mm diameter pin with a load of 1/4 pound can be inserted only 1 mm deep into the surface of a CPC paste, as determined using ISO 1566, a method commonly used for measuring the setting time of dental zinc phosphate cements as well as CPC
- Working time as the term is used herein means the time after which a CPC paste becomes too viscous to be stirred. Generally working time is a few minutes shorter than setting time.
- the CPC paste made by the invention methods has a minimum compressive strength of about 10 MPa and a minimum compressive strength of 25 MPa is obtained within 24 hours after exposure to physiological conditions.
- the compressive strength herein is as determined using ASTM F451-99, a method, that is commonly used for the compressive strength measurement of CPC.
- An injectable formulation of the invention CPC paste can be introduced into a defect in a bone or tooth using any method known in the art and will have working and setting times of about 5 to about 30 minutes. About 30 minutes after introduction into the defect or after exposure to biological conditions, the invention CPC paste will form a substance with a minimum compressive strength of about 10 MPa, or a minimum of 25 MPa compressive strength within 24 hours. Additionally, when solidified, the bone substitute produced from the invention CPC paste can have a porosity of about 20% to about 50% by volume as measured using ASTM C830-00 water saturation technique.
- the CPC paste having these characteristics can consist essentially of calcium phosphate, for example being a substantially monophasic TTCP, and is made from invention particles of monophasic TTCP having surface whiskers or fine needles of calcium phosphate, said whiskers having a length ranging from 1 to about 1000 nm and a width ranging from 1 to about 100 nm as described herein.
- TTCP monophasic particles The most-frequently used wetting agent used in preparation of the invention TTCP monophasic particles is (NH 4 ) HPO 4 with a concentration range 0.1 - 8M, preferably 1 - 6M.
- the length of exposure to the wetting agent will also affect the composition of the particles. For example, when TTCP monophasic particles are treated by exposure to (NH4) 2 HPO 4 for 10 min, the whiskers formed are of monophasic TTCP. However, when the same TTCP monophasic particles are treated by exposure to (NH 4 ) HPO for 24 hours the whiskers become pure hydroxyapatite.
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002520367A CA2520367A1 (en) | 2003-04-16 | 2004-04-16 | Calcium phosphate cement, use and preparation thereof |
EP04750157A EP1613563A1 (en) | 2003-04-16 | 2004-04-16 | Calcium phosphate cement, use and preparation thereof |
AU2004232948A AU2004232948A1 (en) | 2003-04-16 | 2004-04-16 | Calcium phosphate cement, use and preparation thereof |
JP2006510072A JP2007525240A (en) | 2003-04-16 | 2004-04-16 | Calcium phosphate cement and its usage and formulation. |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/414,582 | 2003-04-16 | ||
US10/414,582 US7094282B2 (en) | 2000-07-13 | 2003-04-16 | Calcium phosphate cement, use and preparation thereof |
US10/607,203 | 2003-06-27 | ||
US10/607,023 US6960249B2 (en) | 1999-07-14 | 2003-06-27 | Tetracalcium phosphate (TTCP) having calcium phosphate whisker on surface |
Publications (1)
Publication Number | Publication Date |
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WO2004094335A1 true WO2004094335A1 (en) | 2004-11-04 |
Family
ID=33313093
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US2004/011637 WO2004094335A1 (en) | 2003-04-16 | 2004-04-16 | Calcium phosphate cement, use and preparation thereof |
Country Status (3)
Country | Link |
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US (3) | US6960249B2 (en) |
EP (1) | EP1613563A1 (en) |
WO (1) | WO2004094335A1 (en) |
Cited By (1)
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WO2009096709A2 (en) * | 2008-01-30 | 2009-08-06 | Snu R & Db Foundation | Bone cement with anion |
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US7169373B2 (en) * | 1999-07-14 | 2007-01-30 | Calcitec, Inc. | Tetracalcium phosphate (TTCP) having calcium phosphate whisker on surface and process for preparing the same |
US7094282B2 (en) * | 2000-07-13 | 2006-08-22 | Calcitec, Inc. | Calcium phosphate cement, use and preparation thereof |
US6840995B2 (en) * | 1999-07-14 | 2005-01-11 | Calcitec, Inc. | Process for producing fast-setting, bioresorbable calcium phosphate cements |
US7270705B2 (en) * | 1999-07-14 | 2007-09-18 | Jiin-Huey Chern Lin | Method of increasing working time of tetracalcium phosphate cement paste |
US6960249B2 (en) * | 1999-07-14 | 2005-11-01 | Calcitec, Inc. | Tetracalcium phosphate (TTCP) having calcium phosphate whisker on surface |
US7182928B2 (en) * | 2000-07-13 | 2007-02-27 | Calcitec, Inc. | Calcium phosphate cements made from (TTCP) with surface whiskers and process for preparing same |
US7156915B2 (en) * | 2000-07-13 | 2007-01-02 | Calcitec, Inc. | Tetracalcium phosphate (TTCP) with surface whiskers and method of making same |
US20030216777A1 (en) * | 2002-05-16 | 2003-11-20 | Yin-Chun Tien | Method of enhancing healing of interfacial gap between bone and tendon or ligament |
US7163651B2 (en) * | 2004-02-19 | 2007-01-16 | Calcitec, Inc. | Method for making a porous calcium phosphate article |
US7118705B2 (en) * | 2003-08-05 | 2006-10-10 | Calcitec, Inc. | Method for making a molded calcium phosphate article |
US6994726B2 (en) * | 2004-05-25 | 2006-02-07 | Calcitec, Inc. | Dual function prosthetic bone implant and method for preparing the same |
WO2005046440A2 (en) * | 2003-11-07 | 2005-05-26 | Calcitec, Inc. | Spinal fusion procedure using an injectable bone substitute |
PT1753748E (en) | 2004-05-12 | 2009-08-28 | Pfizer Prod Inc | Proline derivatives and their use as dipeptidyl peptidase iv inhibitors |
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2005
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WO2009096709A2 (en) * | 2008-01-30 | 2009-08-06 | Snu R & Db Foundation | Bone cement with anion |
WO2009096709A3 (en) * | 2008-01-30 | 2009-11-05 | 서울대학교산학협력단 | Bone cement with anion |
Also Published As
Publication number | Publication date |
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EP1613563A1 (en) | 2006-01-11 |
US20050279252A1 (en) | 2005-12-22 |
US20040003757A1 (en) | 2004-01-08 |
US20050268820A1 (en) | 2005-12-08 |
US7160381B2 (en) | 2007-01-09 |
US6960249B2 (en) | 2005-11-01 |
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