Patent US4279812A successfully refreshed from Google Patents.
US4279812A
Expired / Lapsed
US
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Process for preparing macromolecular biologically active collagen
Assignee: Seton Co
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Filing: 1979-09-12
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Granted: 1981-07-21
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Expires: 1999-09-12
Abstract
Abstract Macromolecular reconstituted collagen is prepared by treating natural insoluble collagen with an aqueous solution comprised of an alkali sulfate salt and an alkali metal hydroxide for at least 48 hours to saponify fats suspended within the natural insoluble collagen. The fat free collagen is then treated with an aqueous solution comprised of an alkali metal sulfate for at least four hours to stabilize the interfibular bonds between individual polypeptide chains. The collagen is then dissolved in an aqueous acid solution and frozen at a rate of -20° C./hour. The frozen collagen is vacuum dried at 10 -3 to 10 -5 torr for at least 16 hours to produce a biologically active collagen article. Various biologically active materials may be added to the aqueous acid solution prior to freezing. The collagen product may then be implanted into an animal or the like and the medication slowly released. The article can remain within the biological system and it will slowly dissolve due to enzymatic digestion and through other biological processes.
Inventors
- 👤 Gheorghe Cioca
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 09:36
CPC Classifications
C; C08; C08L; C08L89/00; C08L89/04; C08L89/06; A; A61; A61K; A61K9/00; A61K9/70; A61L; A61L15/00; A61L15/16; A61L15/22; A61L15/32; A61L15/325; A61L15/42; A61L15/44; A61L26/00; A61L26/0009; A61L26/0028; A61L26/0033; A61L2300/00; A61L2300/40; A61L2300/404; A61L2300/43; Y; Y10; Y10S; Y10S128/00; Y10S128/08
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
154 words
A process of preparing macromolecular reconstituted collagen fiber comprising: (a) treating natural insoluble collagen with an aqueous solution comprised of 0.5 to 1 molar of an alkali sulfate salt and 1.0 to 2.5 molar of an alkali metal hydroxide for at least 48 hours and up to 96 hours to saponify fats suspended within the natural insoluble collagen and to uniformly swell the collagen fibers; (b) treating the fat free collagen with an aqueous solution comprised of an alkali metal sulfate for at least four hours to stabilize the interfibular bonds; (c) dissolving the collagen in an aqueous solution; and (d) freezing said solution to effect a temperature reduction rate of -18° C. to -24° C./hour to a temperature of -60° C. to -70° C.; (e) vacuum drying said solution at 10 -3 to 10 -5 torr for at least 12 hours to obtain collagen having an average molecular weight of 383,000 to 460,000.
Claim 2
Dependent Claim
154 words
A process of preparing macromolecular reconstituted collagen fiber comprising: (a) treating natural insoluble collagen with an aqueous solution comprised of 0.5 to 1 molar of an alkali sulfate salt and 1.0 to 2.5 molar of an alkali metal hydroxide for at least 48 hours and up to 96 hours to saponify fats suspended within the natural insoluble collagen and to uniformly swell the collagen fibers; (b) treating the fat free collagen with an aqueous solution comprised of an alkali metal sulfate for at least four hours to stabilize the interfibular bonds; (c) dissolving the collagen in an aqueous solution; and (d) freezing said solution to effect a temperature reduction rate of -18° C. to -24° C./hour to a temperature of -60° C. to -70° C.; (e) vacuum drying said solution at 10 -3 to 10 -5 torr for at least 12 hours to obtain collagen having an average molecular weight of 383,000 to 460,000.
Claim 3
Dependent Claim
24 words
The process according to claim 1 including treating the fat free collagen with distilled water to remove salts therefrom prior to dissolving said collagen.
Claim 4
Dependent Claim
33 words
The process of claim 2 including treating with distilled water for at least 4 hours, decanting the water, and retreating with distilled water at least 4 times for 4 hours for each treatment.
Claim 5
Dependent Claim
13 words
The process according to claim 1 wherein said alkali sulfate is sodium sulfate.
Claim 6
Dependent Claim
13 words
The process of claim 1 wherein said alkali metal hydroxide is sodium hydroxide.
Claim 7
Dependent Claim
25 words
The process of claim 1 wherein said alkali sulfate is present at a level of 0.5 molar to 1.0 molar when stabilizing said interfibular bonds.
Claim 8
Dependent Claim
23 words
The process of claim 1 wherein said collagen is neutralized subsequent to stabilizing the interfibular bonds by washing with an aqueous acid solution.
Claim 9
Dependent Claim
18 words
The process of claim 1 wherein said aqueous solution for dissolving said collagen is an aqueous acid solution.
Claim 10
Dependent Claim
16 words
The process of claim 8 wherein the acid in said aqueous acid solution is ascorbic acid.
Claim 11
Dependent Claim
17 words
The process of claim 9 wherein said aqueous acid solution has a pH of 3 to 4.
Claim 12
Dependent Claim
14 words
The process of claim 1 wherein said natural insoluble collagen is a bovine corium.
Claim 13
Dependent Claim
9 words
The collagen product prepared in accordance with claim 1.
References Cited (Backward Citations)
US2934447A
Cited
US3034852A
Cited
US3157524A
Cited
US3628974A
Cited
US3637642A
Cited
US3514518A
Cited
US3742955A
Cited
US3939831A
Cited
US4097234A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-07-20 | 1985-01-19 | 1985-07-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-07-20 | 1989-01-19 | 1989-07-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-07-20 | 1993-01-19 | 1993-07-21 | $7700.00 | Window Closed / Lapsed |