CA2466001A1 - Bioactive materials, methods of making bioactive materials and method of use thereof - Google Patents
Bioactive materials, methods of making bioactive materials and method of use thereof Download PDFInfo
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- CA2466001A1 CA2466001A1 CA002466001A CA2466001A CA2466001A1 CA 2466001 A1 CA2466001 A1 CA 2466001A1 CA 002466001 A CA002466001 A CA 002466001A CA 2466001 A CA2466001 A CA 2466001A CA 2466001 A1 CA2466001 A1 CA 2466001A1
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- fibroin
- suspension
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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
- A61L27/36—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix
- A61L27/3604—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix characterised by the human or animal origin of the biological material, e.g. hair, fascia, fish scales, silk, shellac, pericardium, pleura, renal tissue, amniotic membrane, parenchymal tissue, fetal tissue, muscle tissue, fat tissue, enamel
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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
- A61L24/0047—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L24/0073—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with a macromolecular matrix
- A61L24/0084—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with a macromolecular matrix containing fillers of phosphorus-containing inorganic compounds, 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
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/0047—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L24/0073—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with a macromolecular matrix
- A61L24/0094—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with a macromolecular matrix containing macromolecular fillers
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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
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/10—Polypeptides; Proteins
- A61L24/108—Specific proteins or polypeptides not covered by groups A61L24/102 - A61L24/106
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0009—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials
- A61L26/0028—Polypeptides; Proteins; Degradation products thereof
- A61L26/0047—Specific proteins or polypeptides not covered by groups A61L26/0033 - A61L26/0042
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0095—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
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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
- A61L27/14—Macromolecular materials
- A61L27/22—Polypeptides or derivatives thereof, e.g. degradation products
- A61L27/227—Other specific proteins or polypeptides not covered by A61L27/222, A61L27/225 or A61L27/24
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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
- A61L27/36—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix
- A61L27/3641—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix characterised by the site of application in the body
- A61L27/3645—Connective tissue
- A61L27/365—Bones
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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
- A61L27/36—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix
- A61L27/38—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix containing added animal cells
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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
- A61L27/36—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix
- A61L27/38—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix containing added animal cells
- A61L27/3839—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix containing added animal cells characterised by the site of application in the body
- A61L27/3843—Connective tissue
- A61L27/3847—Bones
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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
- A61L27/36—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix
- A61L27/38—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix containing added animal cells
- A61L27/3839—Materials for grafts or prostheses or for coating grafts or prostheses containing ingredients of undetermined constitution or reaction products thereof, e.g. transplant tissue, natural bone, extracellular matrix containing added animal cells characterised by the site of application in the body
- A61L27/3843—Connective tissue
- A61L27/3865—Dental/periodontal tissues
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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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/46—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with phosphorus-containing inorganic fillers
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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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/48—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with macromolecular fillers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/02—Drugs for dermatological disorders for treating wounds, ulcers, burns, scars, keloids, or the like
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P19/00—Drugs for skeletal disorders
- A61P19/08—Drugs for skeletal disorders for bone diseases, e.g. rachitism, Paget's disease
- A61P19/10—Drugs for skeletal disorders for bone diseases, e.g. rachitism, Paget's disease for osteoporosis
Abstract
A bioactive material is made using fibroin solutions and suspensions that can be used alone or as a composite with particles such as core/shell particles.
The material is designed to support the constructions, repair, regeneration or augmentation of bone and other tissues of the body. The solutions and suspensions can be loaded with core/shell-type particles comprising inorganic core materials that are coated with biodegradable polymers with an outer coating of a calcium phosphate precursor. The fibroin solutions, suspensions, and composites can be injected to fill cavities or to replace missing tissue.
After injection, the materials can produce a scaffold capable of promoting tissue regeneration while degrading. The degradation of the particles, when present, can generate additional porosity within the scaffold and release other compounds in a controlled manner to enhance growth and activation of the cells necessary for tissue repair. The ability to inject the fibroin solutions, suspensions and composites can reduce the need for many types of surgical procedures that are used to replace or repair bone and other tissues.
The material is designed to support the constructions, repair, regeneration or augmentation of bone and other tissues of the body. The solutions and suspensions can be loaded with core/shell-type particles comprising inorganic core materials that are coated with biodegradable polymers with an outer coating of a calcium phosphate precursor. The fibroin solutions, suspensions, and composites can be injected to fill cavities or to replace missing tissue.
After injection, the materials can produce a scaffold capable of promoting tissue regeneration while degrading. The degradation of the particles, when present, can generate additional porosity within the scaffold and release other compounds in a controlled manner to enhance growth and activation of the cells necessary for tissue repair. The ability to inject the fibroin solutions, suspensions and composites can reduce the need for many types of surgical procedures that are used to replace or repair bone and other tissues.
Claims (27)
1. A composition comprising a fibroin suspension and a pore-forming particulate material.
2. The composition of claim 1, wherein the fibroin suspension is in the form of an occlusion, a gel, a cream or a paste.
3. The composition of Claim 1, wherein the fibroin comprises a Bombyx mori silkworm fibroin.
4. The composition of Claim 1, wherein the fibroin suspension is injectable or implantable.
5. The composition of Claim 1, wherein the pore-forming particulate material comprises a hydroxyapatite, a tricalcium phosphate, a ceramic, a coral, a chitosan, or a combination comprising one or more of the foregoing materials.
6. The composition of Claim 1 wherein the pore-forming particulate material comprises a core-shell particle comprising an optional calcium compound, an optional phosphate source, and an optional reactive layer.
7. The composition of Claim I, wherein the shell comprises a biodegradable polymer.
8. The composition of Claim 6, wherein the core comprises a hydroxyaptatite, a calcium. phosphate-based mineral, a resorbable glass filler, or a combination comprising one or more of the foregoing materials, and wherein the shell comprises polylactic acid, polyglycolic acid, polycaprolactone, polythimethylcarbonate, polyethylene glycol diacrylates, polyanhidrides, polyorthoesters, polyphosphazines, polyacetals, polyesters, polyureas, polycarbonates, polyurethanes, polyalpha-hydroxy acids, polyamides.
polyamino acids, a copolymer, or a combination comprising one or more of the foregoing biodegradable polymers.
polyamino acids, a copolymer, or a combination comprising one or more of the foregoing biodegradable polymers.
9. The composition of Claim I, wherein the fibroin suspension furthcr comprises a physiologically active agent.
The composition of Claim 9, wherein the physiologically active agent comprises cells, antibiotics, bone morphogenetic proteins, compounds that stimulate tissue growth, compounds that stimulate bone regeneration,compounds that stimulate wound repair,or a combination comprising one or more of the foregoing agents
11. A methos for the formation of a fibroin suspension, comprising treating a fibroin solution with an agent comprising heat, an acid, an alcohol, a proteolytic enzyme,a biocompatible polymer, or a combination comprising one or more of the foregoing agents, to form a fibroin suspension;
wherein the fibroin suspension is injectable and bioactive.
wherein the fibroin suspension is injectable and bioactive.
12. The method of Claim 11, wherein, after injection in vivo, the fibroin suspension forms a porous scaffold.
13. The method of Claim 11, wherein the fibroin suspension is in the form of an occlusion, a gel. a cream, or a paste.
14. The method of Claim 11. wherein treating with heat comprises heating to a temperature of about -20°C to about 50 °C.
15. The method of Claim 11, wherein the alcohol comprises glycerol, wherein the acid comprises citric acid, ascorbic acid, lactic acid or a combination comprising one or more of the foregoing acids, wherein the biocompatible polymer comprises polyethylenealycol, polyethyleneoxide, polyvinylpyrrolidone, or a combination comprising one or more of the foregoing biocompatible polymers, and wherein proteolytic enzyme comprises the protease from Streptomyces griseus, papain, chymotrypsin, or a combination comprising one or more of the foregoing proteolytic enzymes.
16. The method of Claim 11, further comprising adding a pore-forming particulate material, a physiologically active agent, or a combination comprising one or more of the foregoing agents anti materials to the fibroin suspension.
17. A method of treating a mammal with a fibroin solution or suspension, comprising administering to a site of tissue construction a fibroin solution or suspension in an amount effective to stimulate tissue formation, wherein the fibroin solution or suspension optionally comprises a pore-forming particulate material, a physiologically active agent, ar a combination comprising one or more of the foregoing agents.
18. The method of Claim 17, wherein the fibroin suspension is in the form of an occlusion, a gel, a cream, or a paste.
19. A method of treating a cell with a fibroin solution or suspension, comprising contacting a cell with a fibroin solution or suspension in an amount effective to induce cell proliferation.
20. The method of Claim 19, wherein the fibroin suspension is in the form of an occlusion, a gel, a cream or a paste.
.
.
21. A composition comprising a fibroin suspension, wherein the suspension is injectable and bioactive.
22. The composition of Claim 21, wherein the after injection in vivo, the fibroin suspension forms a porous scaffold.
23. The composition of claim 21, wherein the fibroin suspension is in the form of an occlusion, a gel a cream or a paste
24. The composition of Claim 21, wherein the fibroin comprises a Bomhyx mori silkworm fibroin.
25- 'The composition of Claim 21, further comprising a physiologically active agent,
26 The composition of Claim. 21, wherein the physiologically active agent comprises cells, antibiotics, bone morghogenetic proteins, compounds that stimulate tissue growth, compounds that stimulate bone regeneration, compounds that stimulate wound repair, or a combination comprising one or more of the foregoing agents.
27. The composition Claim 23, wherein the fibroin gel or occlusion is injectable through an aperture having a diameter of about 584 micrometers, the fibroin cream is injectable through an aperture having a diameter of about 838 micrometers, and the fibroin paste in injectable through an aperature having a diameter of greater than about 2 millimeters.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US34300601P | 2001-10-25 | 2001-10-25 | |
US60/343,006 | 2001-10-25 | ||
PCT/US2002/034252 WO2003035124A2 (en) | 2001-10-25 | 2002-10-25 | Fibroin compositions and methods of making the same |
Publications (2)
Publication Number | Publication Date |
---|---|
CA2466001A1 true CA2466001A1 (en) | 2003-05-01 |
CA2466001C CA2466001C (en) | 2012-01-03 |
Family
ID=23344279
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA2466001A Expired - Fee Related CA2466001C (en) | 2001-10-25 | 2002-10-25 | Bioactive materials, methods of making bioactive materials and method of use thereof |
Country Status (10)
Country | Link |
---|---|
US (3) | US7727542B2 (en) |
EP (1) | EP1446169B1 (en) |
JP (1) | JP4669662B2 (en) |
CN (1) | CN1277584C (en) |
AT (1) | ATE420671T1 (en) |
AU (1) | AU2002348072A1 (en) |
CA (1) | CA2466001C (en) |
DE (1) | DE60230907D1 (en) |
ES (1) | ES2321915T3 (en) |
WO (1) | WO2003035124A2 (en) |
Families Citing this family (69)
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-
2002
- 2002-10-25 WO PCT/US2002/034252 patent/WO2003035124A2/en active Application Filing
- 2002-10-25 ES ES02784287T patent/ES2321915T3/en not_active Expired - Lifetime
- 2002-10-25 DE DE60230907T patent/DE60230907D1/en not_active Expired - Lifetime
- 2002-10-25 JP JP2003537688A patent/JP4669662B2/en not_active Expired - Fee Related
- 2002-10-25 CN CNB028212819A patent/CN1277584C/en not_active Expired - Fee Related
- 2002-10-25 AT AT02784287T patent/ATE420671T1/en not_active IP Right Cessation
- 2002-10-25 AU AU2002348072A patent/AU2002348072A1/en not_active Abandoned
- 2002-10-25 CA CA2466001A patent/CA2466001C/en not_active Expired - Fee Related
- 2002-10-25 EP EP02784287A patent/EP1446169B1/en not_active Expired - Lifetime
- 2002-10-25 US US10/281,096 patent/US7727542B2/en not_active Expired - Fee Related
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- 2007-04-05 US US11/696,802 patent/US8071118B2/en not_active Expired - Fee Related
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AU2002348072A1 (en) | 2003-05-06 |
US20120040907A1 (en) | 2012-02-16 |
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CN1277584C (en) | 2006-10-04 |
CN1575188A (en) | 2005-02-02 |
ATE420671T1 (en) | 2009-01-15 |
EP1446169B1 (en) | 2009-01-14 |
US20030099630A1 (en) | 2003-05-29 |
EP1446169A2 (en) | 2004-08-18 |
DE60230907D1 (en) | 2009-03-05 |
JP4669662B2 (en) | 2011-04-13 |
US8071118B2 (en) | 2011-12-06 |
ES2321915T3 (en) | 2009-06-15 |
US20070190099A1 (en) | 2007-08-16 |
JP2005510268A (en) | 2005-04-21 |
WO2003035124A3 (en) | 2003-09-12 |
WO2003035124A2 (en) | 2003-05-01 |
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