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11. 发明授权

US07745566B2 Methods for the purification of polymers 有权
标题翻译：聚合物纯化方法
公开(公告)号：US07745566B2
公开(公告)日：2010-06-29
申请号：US12017399
申请日：2008-01-22
申请人： Pratibhash Chattopadhyay , Boris Y. Shekunov , K. Adam Gibson
发明人： Pratibhash Chattopadhyay , Boris Y. Shekunov , K. Adam Gibson
IPC分类号： C08F6/00 , C08G65/46
CPC分类号： C08G63/90 , C08G63/08 , C08G65/30 , Y02P20/544
摘要： The present invention provides methods for purifying polymers. In each embodiment of the invention disclosed herein, a supercritical fluid is contacted with an organic solution that includes a polymer to be purified dissolved in an organic solvent. The supercritical fluid extracts the organic solvent from the organic solution. Impurities such as residual monomers and process solvents are removed with the organic solvent and supercritical fluid, thereby purifying the polymer. The methods of the invention are particularly suitable for use in the purification of biodegradable polymers for use in pharmaceutical applications.
摘要翻译：本发明提供了纯化聚合物的方法。在本文公开的本发明的每个实施方案中，将超临界流体与包含要溶解在有机溶剂中的待纯化聚合物的有机溶液接触。超临界流体从有机溶液中萃取有机溶剂。用有机溶剂和超临界流体除去残留单体和工艺溶剂等杂质，从而纯化聚合物。本发明的方法特别适用于纯化用于制药应用的可生物降解的聚合物。

12. 发明授权

US06986846B2 Method and apparatus for enhanced size reduction of particles using supercritical fluid liquefaction of materials 有权
标题翻译：使用超临界流体物质液化来增强颗粒尺寸减小的方法和装置
公开(公告)号：US06986846B2
公开(公告)日：2006-01-17
申请号：US10932559
申请日：2004-09-02
申请人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Jeffrey S. Seitzinger
发明人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Jeffrey S. Seitzinger
IPC分类号： B01D11/02 , A61K9/14
CPC分类号： B01J2/02 , A61K9/1647 , A61K9/1694 , B01D11/0411
摘要： The present invention provides a method and an apparatus for forming particles using supercritical fluid. The method includes the steps of mixing a load material with a first flow of a supercritical fluid in a first mixing chamber having a primary mixing device disposed therein to form a melt, transferring the melt from the first mixing chamber to a second mixing chamber having a secondary mixing device disposed therein, mixing the melt with a second flow of the supercritical fluid in the second mixing chamber to form a lower viscosity melt, expanding the lower viscosity melt across a pressure drop into an expansion chamber that is at a pressure below the critical pressure of the supercritical fluid to convert the supercritical fluid to a gas and thereby precipitate the load material in the form of particles.
摘要翻译：本发明提供使用超临界流体形成颗粒的方法和装置。该方法包括以下步骤：在第一混合室中混合负载材料与超临界流体的第一流，其中设置有初级混合装置以形成熔体，将熔体从第一混合室转移到具有二次混合装置设置在其中，将熔体与第二混合室中的超临界流体的第二流混合，以形成较低粘度的熔体，将较低粘度的熔体在压降范围内膨胀到膨胀室内，该膨胀室的压力低于临界值超临界流体的压力将超临界流体转化为气体，从而使负载材料以颗粒的形式沉淀。

13. 发明申请

US20080286365A1 Method For Producing Solid-Lipid Composite Drug Particles 有权
标题翻译：生产固体脂质复合药物颗粒的方法
公开(公告)号：US20080286365A1
公开(公告)日：2008-11-20
申请号：US12124518
申请日：2008-05-21
申请人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Robert W. Huff
发明人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Robert W. Huff
IPC分类号： A61K9/14 , A61K47/00 , A61P43/00
CPC分类号： A61K9/167 , A61K9/5123 , B01D11/0403 , B01D11/0407 , B01D11/0411 , B01D11/0484 , B01J13/02
摘要： A method of producing solid composite lipid/drug nanoparticles that includes the steps of: (1) dissolving a lipid and a drug in a suitable organic solvent to form a solution; (2) emulsifying the solution in a liquid to form an emulsion having a discontinuous phase of micelles comprising the organic solvent, the drug and the lipid, and a continuous phase comprising the liquid; and (3) contacting the emulsion with a supercritical fluid under conditions suitable to keep the supercritical fluid in a supercritical state, whereby the supercritical fluid extracts the organic solvent from the micelles, causing them to precipitate as organic-solvent free solid composite lipid/drug nanoparticles suspended or dispersed in the liquid.
摘要翻译：一种生产固体复合脂质/药物纳米颗粒的方法，其包括以下步骤：（1）将脂质和药物溶解在合适的有机溶剂中以形成溶液; （2）将溶液乳化在液体中以形成具有包含有机溶剂，药物和脂质的胶束不连续相的乳液和包含液体的连续相; 和（3）在适合于使超临界流体处于超临界状态的条件下使乳液与超临界流体接触，由此超临界流体从胶束中提取有机溶剂，导致它们作为无机溶剂固体复合脂质/药物沉淀悬浮或分散在液体中的纳米颗粒。

14. 发明申请

US20080260852A1 SUPERCRITICAL FLUID EXTRACTION PRODUCED BY IN-LINE HOMOGENIZATION 审中-公开
标题翻译：通过在线均相生产的超临界流体萃取
公开(公告)号：US20080260852A1
公开(公告)日：2008-10-23
申请号：US12017414
申请日：2008-01-22
申请人： Pratibhash Chattopadhyay , Boris Y. Shekunov , K. Adam Gibson
发明人： Pratibhash Chattopadhyay , Boris Y. Shekunov , K. Adam Gibson
IPC分类号： A61K9/14
CPC分类号： A61K9/1647 , A61K9/1694
摘要： A method for producing micro and/or nanoparticles by contacting an emulsion with a supercritical fluid. The method can be used to produce an aqueous suspension of particles that include a drug encapsulated in a polymer. The drug and polymer are dissolved in an organic solvent to form an organic solution. The organic solution is pumped into contact with an aqueous solution in an in-line homogenization device to form an emulsion. Immediately after the emulsion in the in-line homogenization device, the emulsion contacts the supercritical fluid. The supercritical fluid extracts the organic solvent from the oil droplets of the emulsion, causing the drug and polymer to precipitate into the aqueous phase of the emulsion and thereby form an aqueous suspension of particles that include a drug encapsulated in a polymer.
摘要翻译：一种通过使乳液与超临界流体接触来生产微米和/或纳米颗粒的方法。该方法可用于产生包含封装在聚合物中的药物的颗粒水性悬浮液。将药物和聚合物溶解在有机溶剂中以形成有机溶液。将有机溶液泵入与在线均化装置中的水溶液接触以形成乳液。在在线均化装置中的乳液立即之后，乳液接触超临界流体。超临界流体从乳液的油滴中提取有机溶剂，导致药物和聚合物沉淀到乳液的水相中，从而形成包含封装在聚合物中的药物的颗粒水悬浮液。

15. 发明授权

US06998051B2 Particles from supercritical fluid extraction of emulsion 有权
标题翻译：超临界流体萃取乳液颗粒
公开(公告)号：US06998051B2
公开(公告)日：2006-02-14
申请号：US10423492
申请日：2003-04-25
申请人： Pratibhash Chattopadhyay , Boris Y. Shekunov , Jeffrey S. Seitzinger , Robert W. Huff
发明人： Pratibhash Chattopadhyay , Boris Y. Shekunov , Jeffrey S. Seitzinger , Robert W. Huff
IPC分类号： B01D11/00 , B29B9/00 , A61K9/14
CPC分类号： B01D11/0411 , B01J13/02
摘要： A method of producing microparticles and nanoparticles of a solute via the extraction of solvent, having the solute dissolved therein, from an emulsion using a supercritical fluid. The solute to be precipitated is dissolved in the solvent to form a solution, and the solution is dispersed in an immiscible or partially miscible liquid to form an emulsion. The particles are produced via the extraction of the solvent from the emulsion using the supercritical fluid. The process can produce an aqueous suspension of particles that are substantially insoluble in water, and the solvents used in the process to form the emulsion initially can be recovered and recycled.
摘要翻译：通过使用超临界流体从乳液中提取溶质溶解溶剂的方法来生产溶质的微粒和纳米颗粒。待沉淀的溶质溶解在溶剂中以形成溶液，并将溶液分散在不混溶或部分混溶的液体中以形成乳液。通过使用超临界流体从乳液中提取溶剂来生产颗粒。该方法可以产生基本上不溶于水的颗粒的水性悬浮液，并且可以回收和再循环用于形成乳液的方法中使用的溶剂。

16. 发明授权

US06966990B2 Composite particles and method for preparing 有权
标题翻译：复合颗粒及其制备方法
公开(公告)号：US06966990B2
公开(公告)日：2005-11-22
申请号：US10441137
申请日：2003-05-19
申请人： Pratibhash Chattopadhyay , Boris Y. Shekunov , Jeffrey S. Seitzinger , Robert W. Huff
发明人： Pratibhash Chattopadhyay , Boris Y. Shekunov , Jeffrey S. Seitzinger , Robert W. Huff
IPC分类号： B01D11/04 , B01J2/02 , B01J13/02 , B01D11/02
CPC分类号： B01D11/0411 , B01J13/02
摘要： A method for producing composite particles using a supercritical fluid extraction technique on an emulsion. First and second materials (for example; a polymer and a biologically active material) are dissolved or suspended in a preferably solvent to form a solution or dispersion. The solution or dispersion is emulsified in a polar solvent to form an oil-in-water or water-in-oil-in-water emulsion. The emulsion is contacted with a supercritical fluid to extract the solvent. Removal of the solvent by the supercritical fluid from the emulsion supersaturates at least the first material in the solution causing the first material to precipitate out of the solution as composite particles that include both the first and second materials.
摘要翻译：一种使用超临界流体萃取技术在乳液上制备复合颗粒的方法。将第一和第二材料（例如，聚合物和生物活性材料）溶解或悬浮在优选溶剂中以形成溶液或分散体。将溶液或分散体在极性溶剂中乳化以形成水包油或水包油包水乳液。将乳液与超临界流体接触以萃取溶剂。由超临界流体从乳液中除去溶剂至少使溶液中的第一种材料过饱和，导致第一种材料沉淀出溶液，作为包括第一和第二种材料的复合颗粒。

17. 发明授权

US08642091B2 Method for producing solid-lipid composite drug particles 有权
标题翻译：固体 - 脂质复合药物颗粒的制备方法
公开(公告)号：US08642091B2
公开(公告)日：2014-02-04
申请号：US12124518
申请日：2008-05-21
申请人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Robert W. Huff
发明人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Robert W. Huff
IPC分类号： B29B9/00 , A61K9/14 , A61K9/00 , A61K9/16
CPC分类号： A61K9/167 , A61K9/5123 , B01D11/0403 , B01D11/0407 , B01D11/0411 , B01D11/0484 , B01J13/02
摘要： A method of producing solid composite lipid/drug nanoparticles that includes the steps of: (1) dissolving a lipid and a drug in a suitable organic solvent to form a solution; (2) emulsifying the solution in a liquid to form an emulsion having a discontinuous phase of micelles comprising the organic solvent, the drug and the lipid, and a continuous phase comprising the liquid; and (3) contacting the emulsion with a supercritical fluid under conditions suitable to keep the supercritical fluid in a supercritical state, whereby the supercritical fluid extracts the organic solvent from the micelles, causing them to precipitate as organic-solvent free solid composite lipid/drug nanoparticles suspended or dispersed in the liquid.
摘要翻译：一种生产固体复合脂质/药物纳米颗粒的方法，其包括以下步骤：（1）将脂质和药物溶解在合适的有机溶剂中以形成溶液; （2）将溶液乳化在液体中以形成具有包含有机溶剂，药物和脂质的胶束不连续相的乳液和包含液体的连续相; 和（3）在适合于使超临界流体处于超临界状态的条件下使乳液与超临界流体接触，由此超临界流体从胶束中提取有机溶剂，导致它们作为无机溶剂固体复合脂质/药物沉淀悬浮或分散在液体中的纳米颗粒。

18. 发明授权

US08142814B2 Method and apparatus for supercritical fluid assisted particle production 有权
标题翻译：用于超临界流体辅助颗粒生产的方法和装置
公开(公告)号：US08142814B2
公开(公告)日：2012-03-27
申请号：US10541292
申请日：2004-01-30
申请人： Pratibhash Chattopadhyay , Boris Y. Shekunov , Jeffrey S. Seitzinger
发明人： Pratibhash Chattopadhyay , Boris Y. Shekunov , Jeffrey S. Seitzinger
IPC分类号： A61K9/14
CPC分类号： C08J3/16 , A61K9/145 , A61K9/1617 , A61K9/1694 , B01F3/0807 , B01F7/22 , B01F2003/0064 , B01J2/04 , C08J3/02 , C08J2391/00 , Y02P20/544
摘要： The present invention provides an apparatus and methods of producing particles that include a polymer, a wax and/or lipid and, optionally, a biologically active substance. In accordance with the methods of the invention, a load stock including a polymer, a wax and/or a lipid that is a solid at standard temperature and pressure and, optionally, a biologically active substance is provided. The load stock is contacted with a supercritical fluid to form a melt. The melt is contacted with a polar solvent under suitable conditions to form an emulsion. The emulsion is expanded across a pressure drop to form solid particles that include the load stock. The methods and apparatus facilitate the production of very small particles that have a narrow particle size distribution.
摘要翻译：本发明提供了一种生产包括聚合物，蜡和/或脂质以及任选的生物活性物质的颗粒的装置和方法。根据本发明的方法，提供了包含聚合物，蜡和/或在标准温度和压力下为固体的脂质和任选的生物活性物质的负载储备。负载原料与超临界流体接触以形成熔体。在合适的条件下使熔体与极性溶剂接触以形成乳液。乳液在压降下膨胀以形成包括负载原料的固体颗粒。该方法和装置有助于生产具有窄粒度分布的非常小的颗粒。

19. 发明授权

US07767118B2 Nanoparticles from supercritical fluid antisolvent process using particle growth and agglomeration retardants 有权
标题翻译：纳米颗粒超临界流体反溶剂法使用颗粒生长和聚集阻滞剂
公开(公告)号：US07767118B2
公开(公告)日：2010-08-03
申请号：US10531160
申请日：2004-05-28
申请人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Jeffrey S. Seitzinger
发明人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Jeffrey S. Seitzinger
IPC分类号： A61K9/14 , B29B9/00
CPC分类号： A61K9/1694 , A61K9/1635 , A61K9/1641 , A61K9/1647
摘要： The present invention provides a method of forming particles using supercritical fluid (SCF). In accordance with the method, one or more growth retardant compounds having both SCF-philic and SCF-phobic groups are present when one or more solute materials reach a supersaturation point and begin to form particle nuclei. The growth retardant compounds can reduce the particle growth rate, increase the nucleation rate and also prevent particle agglomeration. Preferred growth retardant compounds include sugar acetates and fluorocarbons.
摘要翻译：本发明提供使用超临界流体（SCF）形成颗粒的方法。根据该方法，当一种或多种溶质材料达到过饱和点并开始形成粒子核时，存在一种或多种具有SCF亲和和SCF-疏水基团的生长阻滞化合物。生长阻滞化合物可以降低颗粒生长速率，增加成核速率，并且还可防止颗粒聚集。优选的生长阻滞化合物包括糖醋酸盐和碳氟化合物。

20. 发明授权

US07455797B2 Method and apparatus for producing particles using supercritical fluid 有权
标题翻译：使用超临界流体生产颗粒的方法和装置
公开(公告)号：US07455797B2
公开(公告)日：2008-11-25
申请号：US10789422
申请日：2004-02-27
申请人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Jeffrey S. Seitzinger , Robert Huff
发明人： Boris Y. Shekunov , Pratibhash Chattopadhyay , Jeffrey S. Seitzinger , Robert Huff
IPC分类号： B29B9/00
CPC分类号： B01D11/0407
摘要： The present invention provides a method of producing particles via a supercritical fluid processing technique, an apparatus for carrying out the method and the particles produced thereby. The method includes: (1) providing: a supercritical fluid; a first solvent that is soluble in the supercritical fluid; a second solvent that is substantially insoluble in the supercritical fluid and is at least partially soluble in or miscible with the first solvent; and a solute that is soluble in the first solvent and is substantially insoluble in the second solvent and the supercritical fluid; (2) contacting the first solvent, the second solvent and the solute together to form a solution; and (3) contacting the solution with the supercritical fluid to extract the first solvent from the solution and precipitate the solute in the form of particles that are suspended in the second solvent.
摘要翻译：本发明提供一种通过超临界流体处理技术生产颗粒的方法，用于实施该方法的装置和由其制备的颗粒。该方法包括：（1）提供：超临界流体; 可溶于超临界流体的第一种溶剂; 基本上不溶于超临界流体并且至少部分可溶于第一溶剂或与第一溶剂混溶的第二溶剂; 和溶解在第一溶剂中且基本上不溶于第二溶剂和超临界流体的溶质; （2）将第一溶剂，第二溶剂和溶质接触在一起形成溶液; 和（3）使溶液与超临界流体接触以从溶液中萃取出第一溶剂，并以悬浮在第二溶剂中的颗粒形式沉淀溶质。

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