US5206028A
Expired / Lapsed
US
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Dense collagen membrane matrices for medical uses
Assignee: COLLA-TEC INCORPORATED A CORP OF
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Filing: 1991-02-11
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Granted: 1993-04-27
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Expires: 2011-02-11
Abstract
Abstract The present invention is directed to collagen membranes having physical and biological properties which make them extremely suitable and desirable for all types of medical uses, particularly as a periodontal barrier. The membranes are characterized by having a surface roughness morphology similar to leather and are translucent. Moreover, these membranes do not swell appreciably upon being wetted so as to maintain their overall bulk density. Methods for preparing these membranes and applications for their use are also disclosed.
Inventors
- 👤 Shu-Tung Li
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 19:03
CPC Classifications
A; A61; A61K; A61K9/00; A61K9/0012; A61K9/0053; A61K9/0063; A61K6/00; A61K6/50; A61K6/54
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
222 words
A method of making a dense collagen membranous matrix material which when wetted with water is translucent and non-slippery comprising the steps of: a) forming an aqueous dispersion containing insoluble Type I collagen; b) freezing the aqueous dispersion; c) subjecting the frozen dispersion to freeze-drying conditions to remove frozen water and form a collagen sponge matrix; d) subjecting the collagen membranous matrix to humidification conditions for a time period of about 10 to about 65 minutes, such that the collagen membranous matrix absorbs about 10% to about 30% water by weight based on the weight of the collagen membranous prior to the humidification step; e) compressing the humidified collagen membranous matrix; f) cross-linking the compressed collagen matrix in either a liquid or vapor phase by treatment with a cross-linking agent selected from the group consisting of chromium sulfate, formaldehyde, glutaraldehyde, carbodiimide and adipyl dichloride, by immersing the collagen matrix in a solution of the cross-linking agent and then substantially removing the cross-linking agent; g) refreezing the cross-linked collagen matrix; h) resubjecting the frozen collagen matrix to freeze-drying conditions to remove frozen water; i) resubjecting the dried cross-linked collagen matrix to humidification conditions comprising a for a time period of about 5 to about 30 minutes; and then j) further compressing the humidified, collagen matrix to form the dense collagen membrane matrix material.
Claim 2
Independent Claim
222 words
A method of making a dense collagen membranous matrix material which when wetted with water is translucent and non-slippery comprising the steps of: a) forming an aqueous dispersion containing insoluble Type I collagen; b) freezing the aqueous dispersion; c) subjecting the frozen dispersion to freeze-drying conditions to remove frozen water and form a collagen sponge matrix; d) subjecting the collagen membranous matrix to humidification conditions for a time period of about 10 to about 65 minutes, such that the collagen membranous matrix absorbs about 10% to about 30% water by weight based on the weight of the collagen membranous prior to the humidification step; e) compressing the humidified collagen membranous matrix; f) cross-linking the compressed collagen matrix in either a liquid or vapor phase by treatment with a cross-linking agent selected from the group consisting of chromium sulfate, formaldehyde, glutaraldehyde, carbodiimide and adipyl dichloride, by immersing the collagen matrix in a solution of the cross-linking agent and then substantially removing the cross-linking agent; g) refreezing the cross-linked collagen matrix; h) resubjecting the frozen collagen matrix to freeze-drying conditions to remove frozen water; i) resubjecting the dried cross-linked collagen matrix to humidification conditions comprising a for a time period of about 5 to about 30 minutes; and then j) further compressing the humidified, collagen matrix to form the dense collagen membrane matrix material.
Claim 3
Dependent Claim
15 words
The method of claim 1, wherein the Type I collagen is obtained from bovine tendons.
Claim 4
Dependent Claim
10 words
The method of claim 1, wherein the dispersion contains medicaments.
Claim 5
Dependent Claim
20 words
The method of claim 3, wherein the medicaments include antibiotics, heparin, heparan sulfate proteoglycan glycosaminoglycans epidermal growth factor, and/or glycoproteins.
Claim 6
Dependent Claim
38 words
The method of claim 1, wherein freezing step (b) is carried out at a temperature in the range of from about -10° C. to about -40° C. for a period of from about 1 to about 24 hours.
Claim 7
Dependent Claim
73 words
The method of claim 1, wherein freeze drying step (c) is carried out under by subjecting the frozen dispersion to a vacuum of from about 50 to about 300 microns Hg, at a temperature of from about -10° C. to about -50° C., for a period of about 48 to about 96 hours and then raising the temperature to about 10° C. to about 30° C. for about 10 to about 30 hours.
Claim 8
Dependent Claim
42 words
The method of claim 1, wherein the amount of water absorbed in step (d) is in the range of from about 15% to about 25% water by weight, based on the weight of the collagen membranous matrix prior to the humidification step.
Claim 9
Dependent Claim
32 words
The method of claim 1, wherein the humidification conditions of step (d) include a relative humidity of about 78% to about 94%, and a temperature of about 20° to about 30° C.
Claim 10
Dependent Claim
31 words
The method of claim 1, wherein the humidified collagen membranous matrix is compressed in step (e) to a bulk density in the range of from about 0.5 to about 1.5 g/cc.
Claim 11
Dependent Claim
27 words
The method of claim 9, wherein the collagen membranous matrix is compressed to a bulk density in the range of from about 0.8 to about 1.2 g/cc.
Claim 12
Dependent Claim
31 words
The method of claim 1, wherein the humidified collagen membranous matrix is compressed in step (e) to a thickness in the range of from about 0.15 mm to about 0.25 mm.
Claim 13
Dependent Claim
21 words
The method of claim 11, wherein the thickness is in the range of from about 0.17 mm to about 0.23 mm.
Claim 14
Dependent Claim
32 words
The method of claim 1, wherein the degree of cross-linking is such that the collagen material has a shrink temperature in the range of from about 55° C. to about 75° C.
Claim 15
Dependent Claim
22 words
The method of claim 13, wherein the shrink temperature is in the range of from about 60° C. to about 65° C.
Claim 16
Dependent Claim
25 words
The method of claim 1, wherein the degree of cross-linking is such that the collagen material is resorbed within about 4 to about 7 weeks.
Claim 17
Dependent Claim
34 words
The method of claim 1, wherein freezing step (g) is carried out for about 0.5 to about 12 hours at a temperature in the range of from about -10° C. to about -40° C.
Claim 18
Dependent Claim
66 words
The method of claim 1, wherein freeze-drying step (h) is carried out for about 24 to about 48 hours at a temperature in the range of from about -10° C. to about -50° C., at a vacuum of from about 50 to about 300 microns Hg, and then raising the temperature to about 10° C. to about 30° C. for about 5 to about 15 hours.
Claim 19
Dependent Claim
31 words
The method of claim 1, wherein the humidification conditions of step (i) include a relative humidity of about 78% to about 94%, a temperature of about 20° to about 30° C.
Claim 20
Dependent Claim
40 words
The method of claim 1, wherein the humidification conditions of step (i) are such that the collagen matrix absorbs about 10% to about 30% water by weight, based on the weight of the collagen matrix prior to the humidification step.
Claim 21
Dependent Claim
38 words
The method of claim 19, wherein the about of water absorbed is in the range of from about 15% to about 25% water by weight, based on the weight of the collagen matrix prior to the humidification step.
Claim 22
Dependent Claim
30 words
The method of claim 1, wherein the humidified collagen matrix is compressed in step (j) to a bulk density in the range of from about 0.5 to about 1.5 g/cc.
Claim 23
Dependent Claim
26 words
The method of claim 21, wherein the collagen matrix is compressed to a bulk density in the range of from about 0.8 to about 1.2 g/cc.
Claim 24
Dependent Claim
31 words
The method of claim 1, wherein the humidified collagen membranous matrix is compressed in step (j) to a thickness in the range of from about 0.15 mm to about 0.25 mm.
Claim 25
Dependent Claim
21 words
The method of claim 23, wherein the thickness is in the range of from about 0.17 mm to about 0.23 mm.
Claim 26
Dependent Claim
29 words
The dense collagen membrane matrix material produced by the method of claim 1 having a pore size in the range of from about 0.003 μm to about 0.10 μm.
Claim 27
Dependent Claim
23 words
A dense collagen membrane matrix material made by the method of claim 1 characterized by being translucent and non-slippery when wetted with water.
Claim 28
Dependent Claim
63 words
A dense collage membranous material made by the method of claim 1 having a density of from about 0.5 to about 1.5 g/cc; a rolling resistance of from about 0.15 to about 0.5 mm; a light transmittance of from about 0 to about 10% when fully hydrated; and a pore size in the range of from about 0.003 μm to about 0.10 μm.
Claim 29
Dependent Claim
84 words
A method of treating a patient having periodontitis by surgically exposing the root surface of a tooth, debriding the exposed area and placing a membrane over the debrided root surface so as to prevent epithelium and gingival connective tissue from contacting the root surfaces during healing, the improvement which comprises using a collagen membrane matrix made according to the method of claim 1 having an apparent density of from about 0.5 to about 1.5 g/cc, which when wetted with water is translucent and non-slippery.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1996-04-26 | 1996-10-26 | 1997-04-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-04-26 | 2000-10-26 | 2001-04-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-04-26 | 2004-10-26 | 2005-04-27 | $7700.00 | Window Closed / Lapsed |