US5141747A
Expired / Lapsed
US
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Denatured collagen membrane
Assignee: 3M Co
•
Filing: 1989-05-23
•
Granted: 1992-08-25
•
Expires: 2009-05-23
Abstract
Abstract Disclosed is an artificial membrane comprising a product made by cross-linking molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or combination thereof on the coupler wherein non-coupled lysine epsilon amino groups are bonded to a modifier wherein the modifier is a carbonyl sulfonyl, carbamoyl, or β-malic acid group.
Inventors
- 👤 Matthew T. Scholz
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 15:35
CPC Classifications
A; A61; A61L; A61L27/00; A61L27/14; A61L27/22; A61L27/24; C; C07; C07K; C07K14/00; C07K14/435; C07K14/78; C08; C08H; C08H1/00; C08H1/06; A61F; A61F2/00; A61F2/02; A61F2/18; A61F2310/00; A61F2310/00005; A61F2310/00365; A61K; A61K38/00
Claims Analysis
Total Claims: 43
Claim 1
Independent Claim
64 words
An artificial membrane comprising a product made by cross-linking molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or combination thereof on the coupler wherein non-coupled lysine epsilon amino groups are bonded to a modifier wherein the modifier is selective from the group consisting of a carbonyl, sulfonyl, carbamoyl, or β-malic acid group.
Claim 2
Dependent Claim
64 words
An artificial membrane comprising a product made by cross-linking molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or combination thereof on the coupler wherein non-coupled lysine epsilon amino groups are bonded to a modifier wherein the modifier is selective from the group consisting of a carbonyl, sulfonyl, carbamoyl, or β-malic acid group.
Claim 3
Dependent Claim
36 words
The membrane of claim 1 wherein cross-linking is effected by reacting the molecules with a polyfunctional amine reactive agent selected from the group consisting of a carboxylic acid halide, sulfonyl halide, anhydride, reactive ester, and aldehyde.
Claim 4
Dependent Claim
16 words
The membrane of claim 1 wherein cross-linking is effected by exposing the molecules to actinic radiation.
Claim 5
Dependent Claim
16 words
The membrane of claim 1 wherein cross-linking is effected by dehydrating a gel containing the molecules.
Claim 6
Dependent Claim
24 words
The membrane of claim 1 wherein cross-linking is effected by dehydrating a gel containing the molecules and exposing the dehydrated molecules to actinic radiation.
Claim 7
Dependent Claim
65 words
The membrane of claim 1 wherein the coupler comprises the carbonyl groups, sulfonyl groups, or combination thereof bonded together through an organic radical wherein the organic radical is a C 2-20 saturated or unsaturated aliphatic, aromatic, or aliphatic-aromatic group that is substituted or unsubstituted with halogen or C 1-4 alkyl, alkoxy, or carboxy and has 0-5 heteroatoms wherein the heteroatom is oxygen, sulfur, or nitrogen.
Claim 8
Dependent Claim
24 words
The membrane of claim i wherein the coupler has the formula --CO--CH 2 --CH 2 --CO-- or --CO--CH 2 --CH 2 --CH 2 --CO--.
Claim 9
Dependent Claim
66 words
The membrane of claim 1 wherein the modifier has the formula RCO--, RNHCO--, RSO 2 --, or COOR'CHOHCH(COOR')-- wherein R is a C 2-20 saturated or unsaturated aliphatic, aromatic, or aliphatic-aromatic group that is substituted or unsubstituted with halogen or C 1-4 alkyl, alkoxy, or carboxy and has 0-5 heteroatoms wherein the heteroatom is oxygen, sulfur, or nitrogen and R' is H, Na, K, or Li.
Claim 10
Dependent Claim
12 words
The membrane of claim 8 wherein the modifier has the formula R--NH--CO--.
Claim 11
Dependent Claim
18 words
The membrane of claim 1 wherein the modifier has the formula CH 3 (CH 2 ) 3 --NH--CO--.
Claim 12
Dependent Claim
30 words
The membrane of claim 1 wherein the modifier has the formula CH 3 (CH 2 ) 3 --NH--CO-- and the coupler has the formula --CO-- CH 2 --CH 2 --CO--.
Claim 13
Dependent Claim
27 words
The membrane of claim 1 wherein the molecules were denatured by heating in aqueous media to a temperature between about 40° and 120° C. and thereafter cooling.
Claim 14
Dependent Claim
35 words
An artificial membrane comprising a product made by cross-linking molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or combination thereof on the coupler.
Claim 15
Dependent Claim
35 words
An artificial membrane comprising a product made by cross-linking molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or combination thereof on the coupler.
Claim 16
Dependent Claim
36 words
The membrane of claim 13 wherein cross-linking is effected by reacting the molecules with a polyfunctional amine reactive agent selected from the group consisting of a carboxylic acid halide, sulfonyl halide, anhydride, aldehyde, and reactive ester.
Claim 17
Dependent Claim
16 words
The membrane of claim 13 wherein cross-linking is effected by exposing the molecules to actinic radiation.
Claim 18
Dependent Claim
13 words
The membrane of claim 13 wherein cross-linking is effected by dehydrating the molecules.
Claim 19
Dependent Claim
20 words
The membrane of claim 13 wherein cross-linking is effected by dehydrating the molecules and exposing the molecules to actinic radiation.
Claim 20
Dependent Claim
22 words
The membrane of claim 13 wherein the coupler is --CO--CH 2 --CH 2 --CO-- or --CO--CH 2 --CH 2 --CH 2 --CO--.
Claim 21
Dependent Claim
27 words
The membrane of claim 13 wherein the molecules were denatured by heating in aqueous media to a temperature between about 40° and 120° C. and thereafter cooling.
Claim 22
Independent Claim
101 words
A method for making an artificial membrane comprising the steps of: a) reacting native collagen molecules with a polyfunctional amine-reactive agent selected from the group consisting of a carboxylic acid halide, sulfonyl halide, anhydride, and reactive ester in aqueous media at a pH greater than about 8 and at a temperature between 0° and 35° C. to form coupled collagen molecules; b) heating the coupled collagen molecules at a temperature between about 40° and 120° C. to denature the collagen; c) purifying the coupled collagen molecules; and d) cooling and forming the denatured and coupled collagen molecules into a membranous gel.
Claim 23
Independent Claim
101 words
A method for making an artificial membrane comprising the steps of: a) reacting native collagen molecules with a polyfunctional amine-reactive agent selected from the group consisting of a carboxylic acid halide, sulfonyl halide, anhydride, and reactive ester in aqueous media at a pH greater than about 8 and at a temperature between 0° and 35° C. to form coupled collagen molecules; b) heating the coupled collagen molecules at a temperature between about 40° and 120° C. to denature the collagen; c) purifying the coupled collagen molecules; and d) cooling and forming the denatured and coupled collagen molecules into a membranous gel.
Claim 24
Dependent Claim
19 words
The method of claim 20 further comprising the step of sufficiently dehydrating the gel to cross-link the collagen molecules.
Claim 25
Dependent Claim
42 words
The method of claim 20 further comprising the step of reacting the collagen molecules with a polyfunctional amine-reactive agent selected from the group consisting of a carboxylic acid halide, sulfonyl halide, anhydride, and reactive ester after dehydration and subsequently purifying the product.
Claim 26
Dependent Claim
22 words
The method of claim 20 further comprising the step of exposing the gel to sufficient actinic radiation to cross-link the collagen molecules.
Claim 27
Dependent Claim
29 words
The method of claim 20 further comprising the steps of dehydrating the gel followed by exposing the collagen molecules to sufficient actinic radiation to further cross-link the collagen molecules.
Claim 28
Dependent Claim
23 words
The method of claim 20 wherein the weight ratio of poly-functional amine-reactive agent to native collagen molecules is between about 1:100 and 6:1.
Claim 29
Dependent Claim
19 words
The method of claim 20 wherein the poly-functional amine reactive agent is succinic acid dichloride or glutaric acid dichloride.
Claim 30
Dependent Claim
60 words
The method of claim 20 further comprising the step of reacting the native collagen molecules with a mono-functional amine reactive agent selected from the group consisting of an anhydride, acid halide, sulfonyl halide, active ester, isocyanate, and epoxy succinic acid in aqueous media at a pH greater than about 8 and at a temperature between about 0° and 35° C.
Claim 31
Dependent Claim
19 words
The method of claim 27 further comprising the step of sufficiently dehydrating the gel to cross-link the collagen molecules.
Claim 32
Dependent Claim
43 words
The method of claim 28 further comprising the step of reacting the collagen molecules with a polyfunctional amine-reactive agent selected from the group consisting of a carboxylic acid halide, sulfonyl halide, anhydride, and reactive active ester after dehydration and subsequently purifying the product.
Claim 33
Dependent Claim
22 words
The method of claim 27 further comprising the step of exposing the gel to sufficient actinic radiation to cross-link the collagen molecules
Claim 34
Dependent Claim
29 words
The method of claim 27 further comprising the steps of dehydrating the gel followed by exposing the collagen molecules to sufficient actinic radiation to further cross-link the collagen molecules.
Claim 35
Dependent Claim
13 words
The method of claim 27 wherein the mono-functional amine reactive agent is n-butylisocyanate.
Claim 36
Dependent Claim
14 words
The method of claim 27 wherein the mono-functional amine reactive agent is epoxysuccinic acid.
Claim 37
Dependent Claim
23 words
The method of claim 27 wherein the weight ratio of mono-functional amine-reactive agent to native collagen molecules is between about 1:100 and 10:1.
Claim 38
Dependent Claim
58 words
A composition comprising molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or combination thereof on the coupler wherein non-cross-linked lysine epsilon amino groups are bonded to a modifier wherein the modifier is selective from the group consisting of a carbonyl, sulfonyl, carbamoyl, or β-malic acid group.
Claim 39
Dependent Claim
58 words
A composition comprising molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or combination thereof on the coupler wherein non-cross-linked lysine epsilon amino groups are bonded to a modifier wherein the modifier is selective from the group consisting of a carbonyl, sulfonyl, carbamoyl, or β-malic acid group.
Claim 40
Dependent Claim
29 words
A composition comprising molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or mixture thereof on the coupler.
Claim 41
Dependent Claim
29 words
A composition comprising molecules of interpenetrating denatured collagen coupled at their lysine epsilon amino groups with a coupler through carbonyl groups, sulfonyl groups, or mixture thereof on the coupler.
Claim 42
Dependent Claim
34 words
In a method for repairing the tympanic membrane of a mammal comprising surgically applying an artificial membrane over the tympanic membrane the improvement wherein the artificial membrane comprises the artificial membrane of claim 1.
Claim 43
Dependent Claim
34 words
In a method for repairing the tympanic membrane of a mammal comprising surgically applying an artificial membrane over the tympanic membrane the improvement wherein the artificial membrane comprises the artificial membrane of claim 13.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1995-08-25 | 1996-02-24 | 1996-08-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1999-08-25 | 2000-02-24 | 2000-08-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2003-08-25 | 2004-02-24 | 2004-08-25 | $7700.00 | Window Closed / Lapsed |