logging in or signing up SPRAY-FREEZE DRYING TECHNIQUE robin_vinnu Download Post to : URL : Related Presentations : Share Add to Flag Embed Email Send to Blogs and Networks Add to Channel Uploaded from authorPOINT lite Insert YouTube videos in PowerPont slides with aS Desktop Copy embed code: (To copy code, click on the text box) Embed: URL: Thumbnail: WordPress Embed Customize Embed The presentation is successfully added In Your Favorites. Views: 955 Category: Education License: All Rights Reserved Like it (1) Dislike it (0) Added: October 31, 2010 This Presentation is Public Favorites: 0 Presentation Description No description available. Comments Posting comment... By: shashi.dsc (13 month(s) ago) hello sir, i have see your spray freeze drying ppt. it is very use full for my studies. so please send one copy to my mail ID shashi.dsc@gmail.com Saving..... Post Reply Close Saving..... Edit Comment Close By: ilaradadiya (16 month(s) ago) sir, i see your presentation. it will help to me in study so plzz email me on ilaradadiya@yahoo.in plzz plzz sir sent me as possible as early.. thnk you Saving..... Post Reply Close Saving..... Edit Comment Close By: sakhi111 (17 month(s) ago) sir, i am working as lecturer in pharmacy college can you please send me your presentation so that i will be helpful to my students. my email adr. is pritigkarade@gmail.com Saving..... Post Reply Close Saving..... Edit Comment Close Premium member Presentation Transcript A SEMINAR ON SPRAY-FREEZE DRYING TECHNIQUE : A SEMINAR ON SPRAY-FREEZE DRYING TECHNIQUE BY B. Anil kumar M. Pharm (1st sem) Industrial pharmacy St.Peter’s Institute of Pharmaceutical Sciences Vidyanagar, Hanamkonda, warangal-506001. contents : contents Introduction. Freeze drying process Spray drying process Advantages and disadvantages Spray-freeze drying process Physico-chemical charecterization References Introduction : Introduction A significant number of active pharmaceutical ingredients (APIs) being discovered exhibit expected therapeutic behaviors, but unfortunately have undesirable drug-like properties such as low solubility and poor ADME performance, making formulation into an effective drug product challenging. In fact, more than 40% of the pharmaceutical candidates in the development pipelines are reported to be categorized as poorly soluble. These compounds are classified as biopharmaceutical classification system (BCS) class II for which their maximum bioavailability is limited by their rate of dissolution. Slide 4: Cryogenic technologies such as freeze drying and spray freezing into liquid (SFL) in particular, have lately attracted considerable attention for BCS class II compounds. These processes use cryogen, particularly liquid nitrogen, to form a solid dispersion composed of nano-dispersed domains of API within the hydrophilic polymer matrix. In order to increase universality of unique lyophilization technique in SFL, authors have developed spray freeze-drying (SFD) technique before, which is combined the conventional spray-dryer with freeze-dryer, both equipments are available in market In addition, SFD technique was further improved by adopting four-fluid nozzle (4N) to expand its application in pharmaceutical industry Freeze-drying process : Freeze-drying process Freeze-drying is a widely used process for drying and improving the stability of various pharmaceutical products including: viruses, vaccines, proteins, peptides, or colloidal carriers :liposomes, nanoparticles, nanoemulsions. This process is relatively slow and expensive, it is especially applies only for products having a high added value. Freeze-drying cycle can be divided into three steps: 1. freezing (solidification), 2. primary drying (ice sublimation) and 3. secondary drying (desorption of unfrozen water). Phase diagram : Phase diagram 1.Freezing step : 1.Freezing step During this step, the liquid suspension is cooled, and ice crystals of pure water forms. As the freezing process continues, more and more water contained in the liquid freezes. This results in increasing concentration of the remaining liquid. As the liquid suspension becomes more concentrated, its viscosity increases inducing inhibition of further crystallization. This highly concentrated and viscous liquid solidifies, yielding an amorphous, crystalline, or combined amorphous-crystalline phase. The small percentage of water that remains in the liquid state and does not freeze is called Bound water. 2.Primary drying step : 2.Primary drying step The primary drying stage involves sublimation of ice from the frozen product. In this process, i) heat is transferred from the shelf to the frozen solution through the tray and the vial, and conducted to the sublimation front, ii) the ice sublimes and the water vapor formed passes through the dried portion of the product to the surface of the sample, iii) the water vapor is transferred from the surface of the product through the chamber to the condenser, and iv) the water vapor condenses on the condenser. At the end of sublimation step a porous plug is formed. Its pores correspond to the spaces that were occupied by ice crystals 3.Secondary drying : 3.Secondary drying The primary drying process leaves products with about 0.5% moisture in the solid and this removed in the secondary drying process. The usual method is to raise the temperature, often as high as 50˚C to 60˚C. The secondary drying period is ordinary vacuum drying, the product is virtually free from moisture. Frequently , the secondary drying stage may be started at higher moisture content, often 5% to 2%. Advantages of freeze drying : Advantages of freeze drying Drying takes place at very low temperatures, so that enzyme action is inhibited The solution is frozen, so that the final dry product is a network of solid occupying the same volume as the original solution. The porous form of the product gives ready solubility. There is no concentration of the solution prior to drying. Hence, salts do not concentrate and denature proteins as occur with the other drying methods. Under high vacuum, there is no contact with the air and oxidation is minimised. disadvantages : disadvantages The porosity , ready solubility and complete dryness yields a very hygroscopic product. The process is very slow and uses complicated plant which is very expensive. uses The method is applied only to biological products ex; Antibiotics ( other than penicillin) Blood products Vaccines (such as BCG, yellow fever, smallpox). Enzyme preparations and microbiological cultures. Spray drying : Spray drying The spray drying provides a large surface area for heat and mass transfer by atomising the liquid to small droplets. They are sprayed in to a stream of hot air, so that each droplet dries to a solid particle. spray dried products are easily recognisable, being uniform in appearance . They are in the form of hollow spheres with a small hole. The droplet enters the hot air stream and dries on the outside to form an outer crust with liquid still in the centre. This liquid then vaporises, the vapour escaping by blowing a hole in the sphere. Slide 16: It has been suggested that this method of drying allows a dry product to retain some properties of the feed A droplet from an emulsion dries with the disperse phase inside and a layer of continuous phase on the outside. When reconstituted the emulsion is easily re-formed. The spray drier can be used for drying almost any substance in solution or in suspension. Ex; Borax Citric acid Hexamine Sodium phosphate Gelatin, acacia Starch, barium sulphate and calcium phosphate(insoluble materials) Advantages of the spray drying process : Advantages of the spray drying process The droplets are small, giving a large surface area for heat and mass transfer, so that evaporation is very rapid. Because evaporation is very rapid, the droplets do not attain a high temperature, most of the being used as latent heat of vaporisation. The characteristic particle form gives the product a high bulk density and ready solubility. The product will have a uniform and controllable particle size. Labour costs are low, the process yields a dry free flowing powder. disadvantages : disadvantages The equipment is very bulky and with the ancillary equipment (fans, heaters, separators etc.) is expensive. In a large installation, the drying chamber alone may be as much as 15m in height and 6m in diameter. The thermal efficiency is rather low, since the air must still be hot enough when it leaves the dryer to avoid condensation of moisture. Spray-freeze drying process : Spray-freeze drying process The SFD preparation using 4N is shortly described as “4N-SFD” in this report to distinguish from our conventional SFD using two-fluid nozzle (2N-SFD). Two spray solutions of drug and carrier were separately prepared and supplied to the nozzle part of spray-dryer. Each spray solution was simultaneously atomized by the compressed air and immediately collided and mixed each other at the tip of nozzle edge. Slide 20: The finely splattered mists in the air were trapped into liquid nitrogen and frozen. The iced droplets suspended in liquid nitrogen were transferred into a round-bottom flask and freeze-dried at room temperature until vacuum level decrease to less than 13 Pa. The resultant spray freeze-dried (SFD) composite particles were collected and stored in glass vials in a desiccator at room temperature before the characterization measurement. Spray freeze dryer : Spray freeze dryer Schematic diagram of spray freeze-drying apparatus with four-fluid nozzle (4N-SFD) technique. Key: S1: sample solution (1), S2: sample solution (2), P: pump, N: nozzle, L: liquid nitrogen, C: compressor, V: pressure valve, and F: freeze-dryer. : Schematic diagram of spray freeze-drying apparatus with four-fluid nozzle (4N-SFD) technique. Key: S1: sample solution (1), S2: sample solution (2), P: pump, N: nozzle, L: liquid nitrogen, C: compressor, V: pressure valve, and F: freeze-dryer. Slide 24: Morphological Analysis of SFD Composite Particles Slide 25: 2. Crystalline Analysis of SFD Composite Particles Slide 26: 3. Dissolution Test References : References H. Fessi, J.P. Devissaguet, F. Puisieux, Process for the preparation of dispersible colloidal systems of a substance in the form of nanoparticles. US patent 5, 118, 528, 2 Jun 1992. S. Galindo-Rodriguez, E. Allémann, H. Fessi and E. Doelker, Physicochemical parameters associated with nanoparticle formation in the salting-out, emulsification-diffusion, and nanoprecipitation methods, Pharm. Res. 21 (2004), pp. 1428–1439. R. Oppenheim, Solid colloidal drug delivery systems: nanoparticles, Int. J. Pharm. 8 (1981), pp. 217–234. M.J. Alonso, Nanoparticulate drug carrier technology. In: S. Cohen and H. Bernstein, Editors, Microparticulate Systems for the Delivery of Proteins and Vaccines, Marcel Dekker, New York (1996), pp. 203–242 Slide 29: THANK U You do not have the permission to view this presentation. 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SPRAY-FREEZE DRYING TECHNIQUE robin_vinnu Download Post to : URL : Related Presentations : Share Add to Flag Embed Email Send to Blogs and Networks Add to Channel Uploaded from authorPOINT lite Insert YouTube videos in PowerPont slides with aS Desktop Copy embed code: (To copy code, click on the text box) Embed: URL: Thumbnail: WordPress Embed Customize Embed The presentation is successfully added In Your Favorites. Views: 955 Category: Education License: All Rights Reserved Like it (1) Dislike it (0) Added: October 31, 2010 This Presentation is Public Favorites: 0 Presentation Description No description available. Comments Posting comment... By: shashi.dsc (13 month(s) ago) hello sir, i have see your spray freeze drying ppt. it is very use full for my studies. so please send one copy to my mail ID shashi.dsc@gmail.com Saving..... Post Reply Close Saving..... Edit Comment Close By: ilaradadiya (16 month(s) ago) sir, i see your presentation. it will help to me in study so plzz email me on ilaradadiya@yahoo.in plzz plzz sir sent me as possible as early.. thnk you Saving..... Post Reply Close Saving..... Edit Comment Close By: sakhi111 (17 month(s) ago) sir, i am working as lecturer in pharmacy college can you please send me your presentation so that i will be helpful to my students. my email adr. is pritigkarade@gmail.com Saving..... Post Reply Close Saving..... Edit Comment Close Premium member Presentation Transcript A SEMINAR ON SPRAY-FREEZE DRYING TECHNIQUE : A SEMINAR ON SPRAY-FREEZE DRYING TECHNIQUE BY B. Anil kumar M. Pharm (1st sem) Industrial pharmacy St.Peter’s Institute of Pharmaceutical Sciences Vidyanagar, Hanamkonda, warangal-506001. contents : contents Introduction. Freeze drying process Spray drying process Advantages and disadvantages Spray-freeze drying process Physico-chemical charecterization References Introduction : Introduction A significant number of active pharmaceutical ingredients (APIs) being discovered exhibit expected therapeutic behaviors, but unfortunately have undesirable drug-like properties such as low solubility and poor ADME performance, making formulation into an effective drug product challenging. In fact, more than 40% of the pharmaceutical candidates in the development pipelines are reported to be categorized as poorly soluble. These compounds are classified as biopharmaceutical classification system (BCS) class II for which their maximum bioavailability is limited by their rate of dissolution. Slide 4: Cryogenic technologies such as freeze drying and spray freezing into liquid (SFL) in particular, have lately attracted considerable attention for BCS class II compounds. These processes use cryogen, particularly liquid nitrogen, to form a solid dispersion composed of nano-dispersed domains of API within the hydrophilic polymer matrix. In order to increase universality of unique lyophilization technique in SFL, authors have developed spray freeze-drying (SFD) technique before, which is combined the conventional spray-dryer with freeze-dryer, both equipments are available in market In addition, SFD technique was further improved by adopting four-fluid nozzle (4N) to expand its application in pharmaceutical industry Freeze-drying process : Freeze-drying process Freeze-drying is a widely used process for drying and improving the stability of various pharmaceutical products including: viruses, vaccines, proteins, peptides, or colloidal carriers :liposomes, nanoparticles, nanoemulsions. This process is relatively slow and expensive, it is especially applies only for products having a high added value. Freeze-drying cycle can be divided into three steps: 1. freezing (solidification), 2. primary drying (ice sublimation) and 3. secondary drying (desorption of unfrozen water). Phase diagram : Phase diagram 1.Freezing step : 1.Freezing step During this step, the liquid suspension is cooled, and ice crystals of pure water forms. As the freezing process continues, more and more water contained in the liquid freezes. This results in increasing concentration of the remaining liquid. As the liquid suspension becomes more concentrated, its viscosity increases inducing inhibition of further crystallization. This highly concentrated and viscous liquid solidifies, yielding an amorphous, crystalline, or combined amorphous-crystalline phase. The small percentage of water that remains in the liquid state and does not freeze is called Bound water. 2.Primary drying step : 2.Primary drying step The primary drying stage involves sublimation of ice from the frozen product. In this process, i) heat is transferred from the shelf to the frozen solution through the tray and the vial, and conducted to the sublimation front, ii) the ice sublimes and the water vapor formed passes through the dried portion of the product to the surface of the sample, iii) the water vapor is transferred from the surface of the product through the chamber to the condenser, and iv) the water vapor condenses on the condenser. At the end of sublimation step a porous plug is formed. Its pores correspond to the spaces that were occupied by ice crystals 3.Secondary drying : 3.Secondary drying The primary drying process leaves products with about 0.5% moisture in the solid and this removed in the secondary drying process. The usual method is to raise the temperature, often as high as 50˚C to 60˚C. The secondary drying period is ordinary vacuum drying, the product is virtually free from moisture. Frequently , the secondary drying stage may be started at higher moisture content, often 5% to 2%. Advantages of freeze drying : Advantages of freeze drying Drying takes place at very low temperatures, so that enzyme action is inhibited The solution is frozen, so that the final dry product is a network of solid occupying the same volume as the original solution. The porous form of the product gives ready solubility. There is no concentration of the solution prior to drying. Hence, salts do not concentrate and denature proteins as occur with the other drying methods. Under high vacuum, there is no contact with the air and oxidation is minimised. disadvantages : disadvantages The porosity , ready solubility and complete dryness yields a very hygroscopic product. The process is very slow and uses complicated plant which is very expensive. uses The method is applied only to biological products ex; Antibiotics ( other than penicillin) Blood products Vaccines (such as BCG, yellow fever, smallpox). Enzyme preparations and microbiological cultures. Spray drying : Spray drying The spray drying provides a large surface area for heat and mass transfer by atomising the liquid to small droplets. They are sprayed in to a stream of hot air, so that each droplet dries to a solid particle. spray dried products are easily recognisable, being uniform in appearance . They are in the form of hollow spheres with a small hole. The droplet enters the hot air stream and dries on the outside to form an outer crust with liquid still in the centre. This liquid then vaporises, the vapour escaping by blowing a hole in the sphere. Slide 16: It has been suggested that this method of drying allows a dry product to retain some properties of the feed A droplet from an emulsion dries with the disperse phase inside and a layer of continuous phase on the outside. When reconstituted the emulsion is easily re-formed. The spray drier can be used for drying almost any substance in solution or in suspension. Ex; Borax Citric acid Hexamine Sodium phosphate Gelatin, acacia Starch, barium sulphate and calcium phosphate(insoluble materials) Advantages of the spray drying process : Advantages of the spray drying process The droplets are small, giving a large surface area for heat and mass transfer, so that evaporation is very rapid. Because evaporation is very rapid, the droplets do not attain a high temperature, most of the being used as latent heat of vaporisation. The characteristic particle form gives the product a high bulk density and ready solubility. The product will have a uniform and controllable particle size. Labour costs are low, the process yields a dry free flowing powder. disadvantages : disadvantages The equipment is very bulky and with the ancillary equipment (fans, heaters, separators etc.) is expensive. In a large installation, the drying chamber alone may be as much as 15m in height and 6m in diameter. The thermal efficiency is rather low, since the air must still be hot enough when it leaves the dryer to avoid condensation of moisture. Spray-freeze drying process : Spray-freeze drying process The SFD preparation using 4N is shortly described as “4N-SFD” in this report to distinguish from our conventional SFD using two-fluid nozzle (2N-SFD). Two spray solutions of drug and carrier were separately prepared and supplied to the nozzle part of spray-dryer. Each spray solution was simultaneously atomized by the compressed air and immediately collided and mixed each other at the tip of nozzle edge. Slide 20: The finely splattered mists in the air were trapped into liquid nitrogen and frozen. The iced droplets suspended in liquid nitrogen were transferred into a round-bottom flask and freeze-dried at room temperature until vacuum level decrease to less than 13 Pa. The resultant spray freeze-dried (SFD) composite particles were collected and stored in glass vials in a desiccator at room temperature before the characterization measurement. Spray freeze dryer : Spray freeze dryer Schematic diagram of spray freeze-drying apparatus with four-fluid nozzle (4N-SFD) technique. Key: S1: sample solution (1), S2: sample solution (2), P: pump, N: nozzle, L: liquid nitrogen, C: compressor, V: pressure valve, and F: freeze-dryer. : Schematic diagram of spray freeze-drying apparatus with four-fluid nozzle (4N-SFD) technique. Key: S1: sample solution (1), S2: sample solution (2), P: pump, N: nozzle, L: liquid nitrogen, C: compressor, V: pressure valve, and F: freeze-dryer. Slide 24: Morphological Analysis of SFD Composite Particles Slide 25: 2. Crystalline Analysis of SFD Composite Particles Slide 26: 3. Dissolution Test References : References H. Fessi, J.P. Devissaguet, F. Puisieux, Process for the preparation of dispersible colloidal systems of a substance in the form of nanoparticles. US patent 5, 118, 528, 2 Jun 1992. S. Galindo-Rodriguez, E. Allémann, H. Fessi and E. Doelker, Physicochemical parameters associated with nanoparticle formation in the salting-out, emulsification-diffusion, and nanoprecipitation methods, Pharm. Res. 21 (2004), pp. 1428–1439. R. Oppenheim, Solid colloidal drug delivery systems: nanoparticles, Int. J. Pharm. 8 (1981), pp. 217–234. M.J. Alonso, Nanoparticulate drug carrier technology. In: S. Cohen and H. Bernstein, Editors, Microparticulate Systems for the Delivery of Proteins and Vaccines, Marcel Dekker, New York (1996), pp. 203–242 Slide 29: THANK U