IP Library Granted Patent US 12,491,163
Granted Patent B2
US 12,491,163 · App. 17/327,732 · Granted Dec 9, 2025

Stabilized microcapsules, method of their preparation and uses thereof

Inventors: Ofer Toledano (Kfar Saba, IL); Karine Neimann (Ness Ziona, IL); Danil Finkel-Moiseev (Rehovot, IL); Maya Erlich (Ness Ziona, IL); Dorit Marco (Rehovot, IL)
Assignee: Mayne Pharma LLC
A61K9/4808A61K9/0014A61K9/4841A61K9/4858A61K9/4875A61K9/501A61K9/5084A61K9/5089A61K31/202A61K31/203A61K31/235A61K31/327A61K31/336
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 12,491,163
App. No.
17/327,732
Granted
Dec 9, 2025
Kind
B2
Abstract

The present application is directed to stabilized core-shell microcapsules comprising a core of benzoyl peroxide (BPO) or all trans retinoic acid (ATRA) and a metal-oxide shell; and to pharmaceutical compositions and methods of use thereof.

Claims (23)

1 . A method for treating acne, said method comprising topically administering to a subject in need thereof a pharmaceutical composition comprising microcapsules comprising tretinoin or a pharmaceutically acceptable salt thereof and a pharmaceutically acceptable carrier or excipient,

wherein said microcapsules comprising tretinoin or a pharmaceutically acceptable salt thereof, wherein the tretinoin is the only active agent in said microcapsules;

each comprise a core encapsulated by a shell, wherein said core comprises a dispersion,

wherein said dispersion comprises:

an oil phase comprising tretinoin in a solid form at a concentration of from 17% to 25% w/w in said oil phase; and

optionally at least one phase changing material;

wherein said at least one phase changing material is not liquid at room temperature,

wherein the tretinoin or a pharmaceutically acceptable salt thereof is in an amount of 0.1% by weight of said composition and the composition further comprises microcapsules comprising benzoyl peroxide, wherein the benzoyl peroxide is in an amount of 3% by weight of said composition, wherein the benzoyl peroxide is the only active agent in said microcapsules;

wherein said phase changing material is selected from the group consisting of natural or synthetic paraffin having a molecular formula of C n H 2n+2 , C 10 -C 100 alkane, C 10 -C 100 alkene, C 10 -C 100 alkyne, waxes, aliphatic alcohols having a molecular formula of CH 3 (CH 2 ) n OH, fatty acids having a molecular formula of CH 3 (CH 2 ) n COOH, and any combination thereof, wherein n is an integer from 10 to 100.

2 . The method according to claim 1 , wherein the shell is a silicon dioxide shell.

3 . The method according to claim 1 , wherein the shell is a metal oxide shell.

4 . The method according to claim 3 , wherein a thickness of said metal oxide shell is ranging from 50 nm to 5000 nm according to the energy selective backscattered-detector.

5 . The method according to claim 1 , wherein an average diameter of said microcapsules comprising tretinoin or a pharmaceutically acceptable salt thereof in the range of from 5 micrometers to 50 micrometers according to the energy selective backscattered-detector.

6 . The method according to claim 1 , wherein the microcapsules comprising encapsulated tretinoin provide a dissolution rate of the tretinoin from 5% to 35% weight/h as measured in a medium of 30%:70% v/v mixture of water:isopropyl alcohol at 32° C.

7 . The method according to claim 1 , wherein said microcapsules comprising tretinoin or a pharmaceutically acceptable salt thereof are stable for a period of from 2 weeks to 2 years at room temperature.

8 . The method according to claim 1 , wherein the carrier is in a form of an ointment, a cream, a lotion, an oil, a solution, an emulsion, a gel, a paste, a milk, an aerosol, a powder or a foam.

9 . The method according to claim 1 , wherein the microencapsulation efficiency of the tretinoin is at least 90% by weight, wherein up to 10% by weight of the tretinoin is not encapsulated.

10 . The method according to claim 1 , wherein in said pharmaceutical composition after two weeks of storage at 40° C. and 75% relative humidity a concentration of all-trans 5,6-epoxy retinoic acid is less than 1% by weight of the initial tretinoin amount prior to storage.

11 . The method according to claim 1 , wherein the microcapsules comprising encapsulated tretinoin provide a dissolution rate of the tretinoin from 5% to 35% weight/h as measured in a medium of 30%:70% v/v mixture of water:isopropyl alcohol at 32° C. and wherein the microcapsules comprising encapsulated benzoyl peroxide provide a dissolution rate of the benzoyl peroxide from 10% to 60% weight/h as measured in a medium of 55%:45% mixture of water:acetonitrile at ambient temperature.

12 . The method according to claim 1 , wherein the benzoyl peroxide has microencapsulation efficiency of at least 75% by weight, wherein up to 25% by weight of the benzoyl peroxide is not encapsulated and the tretinoin has microencapsulation efficiency of at least 90% by weight, wherein up to 10% by weight of the tretinoin is not encapsulated.

13 . The method according to claim 1 , wherein in said pharmaceutical composition after two weeks of storage at 40° C. and 75% relative humidity a concentration of all-trans 5,6-epoxy retinoic acid is less than 1% by weight of the initial tretinoin amount prior to storage.

14 . The method according to claim 1 , wherein the benzoyl peroxide has microencapsulation efficiency of at least 85% by weight, wherein up to 15% by weight of the benzoyl peroxide is not encapsulated and the tretinoin has microencapsulation efficiency of at least 90% by weight, wherein up to 10% by weight of the tretinoin is not encapsulated.

15 . The method according to claim 1 , wherein the benzoyl peroxide has microencapsulation efficiency of at least 90% by weight, wherein up to 10% by weight of the tretinoin is not encapsulated, and the tretinoin has microencapsulation efficiency of at least 90% by weight, wherein up to 10% by weight of the tretinoin is not encapsulated.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 18, 2025
From: SOL-GEL TECHNOLOGIES LTD.
To: MAYNE PHARMA LLC
Reel/Frame 071148/0456 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 26, 2021
From: TOLEDANO, OFER; NEIMANN, KARINE; FINKEL-MOISEEV, DANIL; ERLICH, MAYA; MARCO, DORIT
To: SOL-GEL TECHNOLOGIES LTD.
Reel/Frame 056356/0124 →
Continuity (2)
Provisional Application 63028599 · May 22, 2020
Related Publication 20210361583A1 · Nov 25, 2021
References Cited (82)
US 4235872A · Tocker · 1980 [cited by applicant]
US 4670250A · Baker · 1987 [cited by applicant]
US 4970031A · Gotoh · 1990 [cited by applicant]
US 5238714A · Wallace et al. · 1993 [cited by applicant]
US 5401517A · Meyers et al. · 1995 [cited by applicant]
US 5575987A · Kamei et al. · 1996 [cited by applicant]
US 5690923A · DeVringer et al. · 1997 [cited by applicant]
US 6979440B2 · Shefer et al. · 2005 [cited by applicant]
US 7629394B2 · Yan · 2009 [cited by applicant]
US 8617580B2 · Toledano et al. · 2013 [cited by applicant]
US 9107844B2 · Clark et al. · 2015 [cited by applicant]
US 9205395B2 · Yan · 2015 [cited by applicant]
US 9682031B2 · Goldstein et al. · 2017 [cited by applicant]
US 9687465B2 · Sertchook et al. · 2017 [cited by applicant]
US 9868103B2 · Toledano et al. · 2018 [cited by applicant]
US 10420743B2 · Toledano et al. · 2019 [cited by applicant]
US 10512796B2 · Toledano et al. · 2019 [cited by applicant]
US 10525433B2 · Toledano et al. · 2020 [cited by applicant]
US 10653899B2 · Toledano et al. · 2020 [cited by applicant]
US 10688462B2 · Toledano et al. · 2020 [cited by applicant]
US 20020064541A1 · Lapidot et al. · 2002 [cited by applicant]
US 20030157330A1 · Ostafin et al. · 2003 [cited by applicant]
US 20040137031A1 · Seitz et al. · 2004 [cited by applicant]
US 20060003014A1 · Jadhav et al. · 2006 [cited by applicant]
US 20070237724A1 · Abram et al. · 2007 [cited by applicant]
US 20100016443A1 · Toledano et al. · 2010 [cited by applicant]
US 20100029765A1 · Gupta et al. · 2010 [cited by applicant]
US 20100047357A1 · Toledano et al. · 2010 [cited by applicant]
US 20100180464A1 · Laakso et al. · 2010 [cited by applicant]
US 20100255107A1 · Lapidot et al. · 2010 [cited by applicant]
US 20130095185A1 · Toledano et al. · 2013 [cited by applicant]
US 20140186630A1 · Schwantes · 2014 [cited by applicant]
US 20150190372A1 · Djedour · 2015 [cited by applicant]
US 20150328615A1 · Dihora et al. · 2015 [cited by applicant]
US 20170281571A1 · Sertchook et al. · 2017 [cited by applicant]
US 20180117369A1 · Toledano et al. · 2018 [cited by applicant]
US 20180147165A1 · Sertchook et al. · 2018 [cited by applicant]
US 20180207451A1 · Toledano et al. · 2018 [cited by applicant]
US 20180235924A1 · Toledano et al. · 2018 [cited by applicant]
US 20190015366A1 · Toledano et al. · 2019 [cited by applicant]
US 20190015368A1 · Arkin et al. · 2019 [cited by applicant]
US 20190015369A1 · Arkin et al. · 2019 [cited by applicant]
US 20190336464A1 · Toledano et al. · 2019 [cited by applicant]
US 20200114327A1 · Toledano et al. · 2020 [cited by applicant]
US 20200316005A1 · Toledano et al. · 2020 [cited by applicant]
US 20200383927A1 · Toledano et al. · 2020 [cited by applicant]
US 20210007996A1 · Toledano et al. · 2021 [cited by applicant]
US 20210113511A1 · Toledano et al. · 2021 [cited by applicant]
EP 0248531A2 · 1987 [cited by applicant]
IN 1958CHE2007 · 2009 [cited by applicant]
IN 2080CHE2007 · 2009 [cited by applicant]
WO WO1993021764A1 · 1993 [cited by applicant]
WO WO1994020075A1 · 1994 [cited by applicant]
WO WO2003034979A2 · 2003 [cited by applicant]
WO WO2005009604A1 · 2005 [cited by applicant]
WO WO2007015243A2 · 2007 [cited by applicant]
WO WO2008093346A2 · 2008 [cited by applicant]
WO WO2008093347A2 · 2008 [cited by applicant]
WO WO2009051839A1 · 2009 [cited by applicant]
WO WO2010013250A2 · 2010 [cited by applicant]
WO WO2011080741A2 · 2011 [cited by applicant]
WO WO2013001536A1 · 2013 [cited by applicant]
WO WO2015092602A1 · 2015 [cited by applicant]
WO WO2019012536A1 · 2019 [cited by applicant]
WO WO2019012537A1 · 2019 [cited by applicant]
Binks, B. P. et al. (2005). Nanoparticle silica-stabilised oil-in-water emulsions: improving emulsion stability. [cited by applicant]
Del Rosso, J. Q. et al. (2010). Absence of degradation of tretinoin when benzoyl peroxide is combined with an optimized formulation of tretinoin gel (0.05%). [cited by applicant]
He, J. et al. (2003). Preparation of porous and nonporous silica nanofilms from aqueous sodium silicate. [cited by applicant]
Patel, V. B. et al. (2001). Clinical assessment of the combination therapy with liposomal gels of tretinoin and benzoyl peroxide in acne. [cited by applicant]
Shen, S. L. et al. (2007). A novel process to synthesize magnetic hollow silica microspheres. [cited by applicant]
Skapin, S. D. et al. (2004). Preparation and coating of finely dispersed drugs: 4. Loratadine and danazol. [cited by applicant]
Tjandra, W. et al. (2006). Interaction between silicates and ionic surfactants in dilute solution. [cited by applicant]
Falls, A. H. et al. (1983). A transmission electron microscopy study of hexagonal ice. [cited by applicant]
Gollnick, H. et al. (2003). Management of acne: a report from a Global Alliance to Improve Outcomes in Acne. [cited by applicant]
Koifman, N. A. et al. (2017). A direct-imaging cryo-EM study of shedding extracellular vesicles from leukemic monocytes. [cited by applicant]
Talmon, Y. et al. (1986). Electron beam radiation damage to organic inclusions in vitreous, cubic, and hexagonal ice. [cited by applicant]
Tanghetti, E. (2008). The evolution of benzoyl peroxide therapy. [cited by applicant]
Yan, A. C. (2006). Current concepts in acne management. [cited by applicant]
Yue, P. F. et al. (2009). The study on the entrapment efficiency and in vitro release of puerarin submicron emulsion. [cited by applicant]
Rapini R. P., et al. (2007). Dermatology: 2-Volume Set. St. Louis: Mosby. Section 6, Adnexal Diseases, Webster G. F. Rosacea and Related Disorders, pp. 509-5016. [cited by applicant]
William D. J. et al. (2011). Andrew's Diseases of the Skin, 11th ed., Chapter 13, Rosacea, pp. 241-244. [cited by applicant]
Graber E. (2016, updated 2023). Acne vulgaris: Overview of management, Wolters Kluwer, UpToDate.com, pp. 1-21. Retrieved online at URL: https://www.medilib.ir/uptodate/show/42. [cited by applicant]