IP Library Granted Patent US 7,897,553
Granted Patent B2
US 7,897,553 · App. 11/865,746 · Granted Mar 1, 2011

Biguanide composition with low terminal amine

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Quick Facts
Patent No.
US 7,897,553
App. No.
11/865,746
Granted
Mar 1, 2011
Kind
B2
Abstract

A polymeric biguanide composition comprising less than 18 mol % of terminal amine groups as measured by 13 C NMR. The polymeric biguanide composition also is characterized by a relative increase in the molar concentration of terminal guanidine groups or terminal cyanoguanidino groups. The invention is also directed to ophthalmic compositions comprising the polymeric biguanide compositions. The polymeric biguanide compositions can be used as an antimicrobial component in an ophthalmic lens care solution, or as a preservative to in a pharmaceutical composition or other health care product.

Claims (51)

1. A polymeric biguanide composition comprising less than 18 mol % of terminal amine groups, and 55 mol % or greater of terminal guanidine groups as measured by 13 C NMR, the composition comprising polymeric biguanides of formula (1) and formula (2)

wherein the polymeric biguanides of formula (1) and formula (2) account for at least 80 mol % of the total moles of polymeric biguanides in the composition, wherein

and each TG is the same or different and is selected from CG or G;

R 1 , R 2 and R 3 are divalent radicals of an aliphatic hydrocarbon independently selected from the group consisting of a C 3 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene;

R 4 is selected from the group consisting of a C 2 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene; and

n and m represent a number average of repeat units between 1 and 20.

2. The polymeric biguanide composition of claim 1 comprising less than 15 mol % of terminal amine groups, and 60 mol % or greater of terminal guanidine groups.

3. The polymeric biguanide composition of claim 2 comprising 65 mol % or greater of terminal guanidine groups.

4. The polymeric biguanide composition of claim 1 comprising less than 10 mol % of terminal amine groups.

5. The polymeric biguanide composition of claim 1 comprising polymeric biguanides of formula (1), formula (2), formula (3) and optionally formula (4), and having a molar ratio of

[mol % formula (1) +mol % formula (2)]:[mol % formula (3) +mol % formula (4)] from 70:30 or greater

wherein

and each TG is the same or different and is selected from CG or G;

R 1 , R 2 and R 3 are divalent radicals of an aliphatic hydrocarbon independently selected from the group consisting of a C 3 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene;

R 4 is selected from the group consisting of a C 2 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene;

n represents a number average of repeat units between 1 and 20; and

m is independently selected for each of formulas (2), (3) and (4) and represents a number average of repeat units between 1 and 20.

6. The polymeric biguanide composition of claim 1 wherein the polymeric biguanides of formula (1) and formula (2) account for at least 90 mol % of the total moles of polymeric biguanides.

7. The polymeric biguanide composition of claim 5 wherein n<m.

8. The polymeric biguanide composition of claim 1 wherein n<m.

9. A polymeric biguanide composition comprising less than 18 mol % of terminal amine groups and 40 mol % or greater of terminal cyanoguanidino groups as measured by 13 C NMR, wherein the composition of polymeric biguanides include formula (1) and formula (2)

wherein the polymeric biguanides of formula (1) and formula (2) account for at least 80 mol % of the polymeric biguanides in the composition, wherein

and each TG is the same or different and is selected from CG or G;

R 1 , R, and R 3 are divalent radicals of an aliphatic hydrocarbon independently selected from the group consisting of a C 3 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene;

R 4 is selected from the group consisting of a C 2 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene; and

n and m represent a number average of repeat units between 1 and 20.

10. The polymeric biguanide composition of claim 9 comprising less than 15 mol % of terminal amine groups and 50 mol % or greater of terminal cyanoguanidino groups.

11. The polymeric biguanide composition of claim 9 further comprising from 10 mol % to 30 mol % of terminal guanidine groups.

12. The polymeric biguanide composition of claim 11 comprising 7 to 15 mol % of terminal amine groups and 45 mol% to 70 mol% terminal cyanoguanidino groups.

13. The polymeric biguanide composition of claim 9 further comprising an in-chain biguanide concentration of 90 mol % or greater.

14. An ophthalmic composition comprising one or more cationic antimicrobial components at least one of which is a polymeric biguanide composition that comprises less than 18 mol % of terminal amine groups, and 55 mol % or greater of terminal guanidine groups as measured by 13 C NMR, the composition comprising polymeric biguanides of formula (1) and formula (2)

wherein the polymeric biguanides of formula (1) and formula (2) account for at least 80 mol % of the total moles of polymeric biguanides in the composition, wherein

and each TG is the same or different and is selected from CG or G.

R 1 , R 2 and R 3 are divalent radicals of an aliphatic hydrocarbon independently selected from the group consisting of a C 3 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene;

R 4 is selected from the group consisting of a C 2 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene; and

n and m represent a number average of repeat units between 1 and 20.

15. The ophthalmic composition of claim 14 wherein the polymeric biguanide composition comprises less than 15 mol % of terminal amine groups and 60 mol % or greater of terminal guanidine groups.

16. The ophthalmic composition of claim 15 wherein the polymeric biguanide composition comprises less than 10 mol % of terminal amine groups.

17. The ophthalmic composition of claim 14 further comprising a cationic antimicrobial component selected from the group consisting of poly[dimethylimino-2-butene-1,4-diyl]chloride, α-[4-tris(2-hydroxyethyl) ammonium chloride-2-butenyl]poly[1-dimethylammonium chloride-2-butenyl]-ω-tris(2-hydroxyethyl)ammonium chloride, myristamidopropyl dimethylamine and mixtures thereof.

18. The ophthalmic composition of claim 14 further comprising dexpanthenol, sorbitol or any combination thereof.

19. An ophthalmic composition comprising one or more cationic antimicrobial components at least one of which is a polymeric biguanide composition that comprises less than 18 mol % of terminal amine groups and 40 mol % or greater of terminal cyanoguanidino groups as measured by 13 C NMR, wherein the composition of polymeric biguanides include formula (1) and formula (2)

wherein the polymeric biguanides of formula (1) and formula (2) account for at least 80 mol % of the polymeric biguanides in the composition, wherein

and each TG is the same or different and is selected from CG or G;

R 1 , R 2 , and R 3 are divalent radicals of an aliphatic hydrocarbon independently selected from the group consisting of a C 3 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene;

R 4 is selected from the group consisting of a C 2 -C 12 alkylene, C 4 -C 12 oxyalkylene and C 4 -C 12 thioalkylene; and

n and m represent a number average of repeat units between 1 and 20.

20. The ophthalmic composition of claim 19 wherein the polymeric biguanide composition comprises less than 15 mol % of terminal amine groups and 50 mol % or greater of terminal cyanoguanidino groups.

21. The ophthalmic composition of claim 19 wherein the polymeric biguanide composition comprises from 10 mol % to 30 mol % of terminal guanidine groups.

22. The ophthalmic composition of claim 20 wherein the polymeric biguanide composition comprises 7 to 15mol % of terminal amine groups and 45 mol % to 70 mol % terminal cyanoguanidino groups.

23. The ophthalmic composition of claim 19 further comprising a cationic antimicrobial component selected from the group consisting of poly[dimethylimino-2-butene-1,4-diyl]chloride, α-[4-tris(2-hydroxyethyl) ammonium chloride-2-butenyl]poly[1-dimethylammonium chloride-2-butenyl]-ω-tris(2-hydroxyethyl)ammonium chloride, myristamidopropyl dimethylamine and mixtures thereof.

24. The ophthalmic composition of claim 19 further comprising dexpanthenol, sorbitol or any combination thereof.

Assignments (12)
RELEASE OF SECURITY INTEREST Recorded Nov 20, 2025
From: THE BANK OF NEW YORK MELLON, AS NOTES COLLATERAL AGENT
To: ATON PHARMA, INC.; BAUSCH & LOMB INCORPORATED; BAUSCH & LOMB PHARMA HOLDINGS CORP.; COMMONWEALTH LABORATORIES, LLC; DOW PHARMACEUTICAL SCIENCES, INC.; ECR PHARMACEUTICALS CO., INC.; LABORATOIRE CHAUVIN S.A.S.; MEDICIS PHARMACEUTICAL CORPORATION; ONPHARMA INC.; ORAPHARMA, INC.; PRECISION DERMATOLOGY, INC.; SALIX PHARMACEUTICALS, LTD.; SALIX PHARMACEUTICALS, INC.; SANTARUS, INC.; SOLTA MEDICAL, INC.; SYNERGETICS USA, INC.; TECHNOLAS PERFECT VISION GMBH; VALEANT CANADA LP; VALEANT PHARMACEUTICALS INTERNATIONAL; VALEANT PHARMACEUTICALS INTERNATIONAL, INC.; VALEANT PHARMACEUTICALS NORTH AMERICA LLC; WIRRA IP PTY LIMITED; VALEANT PHARMA POLAND SP. Z O.O.; VALEANT PHARMACEUTICALS LUXEMBOURG S.A R.L.; VALEANT PHARMACEUTICALS IRELAND LIMITED
Reel/Frame 073637/0001 →
RELEASE OF SECURITY INTEREST Recorded Apr 8, 2025
From: BARCLAYS BANK PLC, AS COLLATERAL AGENT
To: SOLTA MEDICAL, INC.; PRECISION DERMATOLOGY, INC.; BAUSCH HEALTH IRELAND LIMITED (F/K/A/ VALEANT PHARMACEUTICALS IRELAND LIMITED); SALIX PHARMACEUTICALS, INC.; SALIX PHARMACEUTICALS, LTD; SANTARUS, INC.; MEDICIS PHARMACEUTICAL CORPORATION; HUMAX PHARMACEUTICAL S.A.; SOLTA MEDICAL IRELAND LIMITED; BAUSCH & LOMB MEXICO, S.A. DE C.V.; BAUSCH+LOMB OPS B.V.; BAUSCH HEALTH AMERICAS, INC.; BAUSCH HEALTH COMPANIES INC.; BAUSCH HEALTH HOLDCO LIMITED; BAUSCH HEALTH MAGYARORSZAG KFT (A/K/A BAUSCH HEALTH HUNGARY LLC); BAUSCH HEALTH POLAND SPOLKA Z OGRANICZONA ODPOWIEDZIALNOSCIA (F/K/A VALEANT PHARMA POLAND SPOLKA Z OGRANICZONA ODPOWIEDZIALNOSCIA); BAUSCH HEALTH US, LLC; BAUSCH HEALTH, CANADA INC. / SANTE BAUSCH, CANADA INC.; ICN POLFA RZESZOW SPOLKA AKCYJNA (A/K/A ICN POLFA RZESZOW S.A.); ORAPHARMA, INC.; PRZEDSIEBIORSTWO FARMACEUTYCZNE JELFA SPOLKA AKCYJNA (A/K/A PRZEDSIEBIORSTWO FARMACEUTYCZNE JELFA S.A.); SOLTA MEDICAL DUTCH HOLDINGS B.V.; V-BAC HOLDING CORP.; VRX HOLDCO LLC; 1261229 B.C. LTD.; 1530065 B.C. LTD.
Reel/Frame 070778/0199 →
OMNIBUS PATENT SECURITY RELEASE AGREEMENT (REEL/FRAME 045444/0634) Recorded Nov 2, 2022
From: THE BANK OF NEW YORK MELLON
To: BAUSCH & LOMB INCORPORATED; LABORATOIRE CHAUVIN S.A.S.; TECHNOLAS PERFECT VISION GMBH; THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES
Reel/Frame 061872/0295 →
RELEASE OF SECURITY INTEREST IN SPECIFIED PATENTS (REEL/FRAME 045444/0299) Recorded Oct 26, 2022
From: BARCLAYS BANK PLC
To: BAUSCH & LOMB INCORPORATED; TECHNOLAS PERFECT VISION GMBH; THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES; PF CONSUMER HEALTHCARE 1 LLC; LABORATOIRE CHAUVIN S.A.S.
Reel/Frame 061779/0001 →
SECURITY INTEREST Recorded Feb 26, 2018
From: ATON PHARMA, INC.; BAUSCH & LOMB INCORPORATED; BAUSCH & LOMB PHARMA HOLDINGS CORP.; COMMONWEALTH LABORATORIES, LLC; DOW PHARMACEUTICAL SCIENCES, INC.; ECR PHARMACEUTICALS CO., INC.; LABORATOIRE CHAUVIN S.A.S.; MEDICIS PHARMACEUTICAL CORPORATION; ONPHARMA INC.; ORAPHARMA, INC.; PRECISION DERMATOLOGY, INC.; SALIX PHARMACEUTICALS, LTD.; SALIX PHARMACEUTICALS, INC.; SANTARUS, INC.; SOLTA MEDICAL, INC.; SYNERGETICS USA, INC.; TECHNOLAS PERFECT VISION GMBH; VALEANT CANADA LP; VALEANT PHARMACEUTICALS INTERNATIONAL; VALEANT PHARMACEUTICALS INTERNATIONAL, INC.; VALEANT PHARMACEUTICALS NORTH AMERICA LLC; WIRRA IP PTY LIMITED; VALEANT PHARMA POLAND SP. Z O.O.; VALEANT PHARMACEUTICALS LUXEMBOURG S.A R.L.; VALEANT PHARMACEUTICALS IRELAND LIMITED
To: BARCLAYS BANK PLC, AS COLLATERAL AGENT
Reel/Frame 045444/0299 →
SECURITY INTEREST Recorded Feb 26, 2018
From: ATON PHARMA, INC.; BAUSCH & LOMB INCORPORATED; BAUSCH & LOMB PHARMA HOLDINGS CORP.; COMMONWEALTH LABORATORIES, LLC; DOW PHARMACEUTICAL SCIENCES, INC.; ECR PHARMACEUTICALS CO., INC.; LABORATOIRE CHAUVIN S.A.S.; MEDICIS PHARMACEUTICAL CORPORATION; ONPHARMA INC.; ORAPHARMA, INC.; PRECISION DERMATOLOGY, INC.; SALIX PHARMACEUTICALS, LTD.; SALIX PHARMACEUTICALS, INC.; SANTARUS, INC.; SOLTA MEDICAL, INC.; SYNERGETICS USA, INC.; TECHNOLAS PERFECT VISION GMBH; VALEANT CANADA LP; VALEANT PHARMACEUTICALS INTERNATIONAL; VALEANT PHARMACEUTICALS INTERNATIONAL, INC.; VALEANT PHARMACEUTICALS NORTH AMERICA LLC; WIRRA IP PTY LIMITED; VALEANT PHARMA POLAND SP. Z O.O.; VALEANT PHARMACEUTICALS LUXEMBOURG S.A R.L.; VALEANT PHARMACEUTICALS IRELAND LIMITED
To: THE BANK OF NEW YORK MELLON, AS COLLATERAL AGENT
Reel/Frame 045444/0634 →
SECURITY INTEREST Recorded Jul 19, 2017
From: BAUSCH & LOMB INCORPORATED
To: THE BANK OF NEW YORK MELLON
Reel/Frame 043251/0932 →
NOTICE OF SUCCESSION OF AGENCY Recorded Jan 9, 2015
From: GOLDMAN SACHS LENDING PARTNERS, LLC
To: BARCLAYS BANK PLC, AS SUCCESSOR AGENT
Reel/Frame 034749/0689 →
SECURITY AGREEMENT Recorded Sep 4, 2013
From: BAUSCH & LOMB INCORPORATED
To: GOLDMAN SACHS LENDING PARTNERS LLC, AS COLLATERAL AGENT
Reel/Frame 031156/0508 →
RELEASE OF SECURITY INTEREST Recorded Aug 13, 2013
From: CITIBANK N.A., AS ADMINISTRATIVE AGENT
To: WP PRISM INC. (N/K/A BAUSCH & LOMB HOLDINGS INC.); BAUSCH & LOMB INCORPORATED; ISTA PHARMACEUTICALS
Reel/Frame 030995/0444 →
SECURITY AGREEMENT Recorded Aug 6, 2012
From: BAUSCH & LOMB INCORPORATED; EYEONICS, INC.
To: CITIBANK N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 028728/0645 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 2, 2007
From: HEILER, DAVID J.
To: BAUSCH & LOMB INCORPORATED
Reel/Frame 019905/0425 →