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WO2011154014A1 - Séchage contrôlé de l'humidité - Google Patents

Séchage contrôlé de l'humidité Download PDF

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Publication number
WO2011154014A1
WO2011154014A1 PCT/DK2011/050209 DK2011050209W WO2011154014A1 WO 2011154014 A1 WO2011154014 A1 WO 2011154014A1 DK 2011050209 W DK2011050209 W DK 2011050209W WO 2011154014 A1 WO2011154014 A1 WO 2011154014A1
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WO
WIPO (PCT)
Prior art keywords
process according
solvent
drying
drying gas
vol
Prior art date
Application number
PCT/DK2011/050209
Other languages
English (en)
Inventor
Henrik Schwartzbach
Andrew P. Birkmire
Original Assignee
Gea Process Engineering A/S
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Gea Process Engineering A/S filed Critical Gea Process Engineering A/S
Publication of WO2011154014A1 publication Critical patent/WO2011154014A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1682—Processes
    • A61K9/1688—Processes resulting in pure drug agglomerate optionally containing up to 5% of excipient

Definitions

  • the present invention relates to a process for preparation of spray dried particles, wherein the humidity is controlled during the proc- ess.
  • a liquid feedstock is atomized into a spray of droplets, which are contacted with hot air in a drying chamber. Evaporation of moisture from the droplets and formation of the desired product as dry particles proceed under controlled tempera- ture and airflow conditions.
  • a powder of the product is continuously discharged from the drying chamber and/or recovered from the exhaust gases using a cyclone or a bag filter. Generally, the entire spray drying process only endures for a few seconds.
  • vapours in the drying gas results from a combination of the vapour pressure in the inlet gas and that of the evaporated solvent(s) from the product.
  • vapour content and composition is given by the solvent evaporated from the product.
  • the inlet drying gas humidity is typically kept as low as economically feasible to obtain a high drying capacity. Drying plants using air as drying gas are frequently equipped with dehumidifiers to control the inlet drying gas humidity. However, few have explored the possibilities of generating special product characteristics by increasing the solvent vapors in the drying gas above the optimal level from the perspective of drying economy.
  • US 7,469,488 discloses spray dried particles having specified aerodynamic characteristics.
  • the particles are produced by atomizing a liquid feed in a drying gas having a controlled humidity.
  • By controlling the humidity of the inlet drying gas to a certain dew point between -39°C and 8°C particles with a specified de- termined tap density or aerodynamic diameter is produced.
  • the object of the present invention is to provide a spray drying process, wherein a detailed vapor control is made possible, thereby generating product characteristics different from prod- uct characteristics produced using the most economic method.
  • a process for the preparation of spray dried particles, said process comprising the steps of spraying in a chamber a liquid feed comprising one or more solvents and suspended and/or dissolved component(s), and supplying a drying gas to the chamber, said drying gas comprising one or more solvent vapours, each having a certain dew point, thereby producing spray dried particles; wherein the dew point is selected to provide a desired property of the spray dried particles.
  • the drying gas may comprise any amount of solvent vapours up to an amount corresponding to 100% relative humidity.
  • the amount of humidity in the inlet drying gas(ses) is above the level corresponding to 10% relative humidity if calculated at the temperatures and pressures at the outlet of the drying chamber, such as above 20%.
  • solvent is used for any volatile component in the product or drying gas supplied to the drying chamber, whether the solvent is organic, non-organic or water. Similar the term vapour refers to this phase for any solvent. The same applies for the term humidity and relative humidity.
  • gas is used for all components that appear in their gaseous form, e.g. nitrogen, carbon dioxide, air etc. throughout the process.
  • the maximum water content in most products from spray drying have to be limited, typically to below 2-5% w/w.
  • the maximum level is usually lower (typically ⁇ 0.5% w/w), e.g. due to health reasons.
  • the required residual solvent levels are frequently achieved through a post drying stage. By increasing the drying temperature, the end point of drying can be driven closer towards zero content of residual solvent in the product and/or the drying time can be reduced.
  • the last op- tion of lowering the vapour pressure in the drying gas is especially used whenever there is an upper limit to the drying temperature (e.g. due to temperature related product deterioration) preventing the residual solvent goal to be reached simply by increasing the drying temperature.
  • the morphology as well as the chemical composition of the final product will depend on the drying gas temperature, the rate of drying as well as the ratio between the different solvents, if more than one is present.
  • the present invention suggests a method for ob- taining the desired characteristics of the dried particles.
  • drying at low temperature may encourage drying off one more problematic solvent (e.g. an organic solvent) at the expense of the drying of a less problematic one (e.g. water). Drying at low temperature at the outlet of the drying chamber, e.g . below 40 °C or more preferred below 20 °C, will result in high relative humidities in the drying gas due to evaporation of liquid. The same will happen when drying at elevated pressure. In any event, some sort of post drying after spray drying may be considered due to the short residence time in the spray dryer.
  • one more problematic solvent e.g. an organic solvent
  • a less problematic one e.g. water
  • a high drying gas temperature may have negative effects on spray dried powders, e.g. the density of the powder, by promoting the formation of unwanted hollow particles.
  • Increasing the drying gas humidity has the opposite effect on the drying rate of the particles and will allow the particles to shrink more during drying. In this way, more fa- vourable properties of the particles are achieved as expressed by common parameters within the art such as tap density, volume median geometric diameter (VMGD), and mass median aerodynamic diameter (MMAD).
  • tap density volume median geometric diameter
  • MMAD mass median aerodynamic diameter
  • the vapour phase composition of the drying gas can be con- trolled by selective removal of vapours from the drying gas prior to its entering the dryer and/or by addition of vapours to the drying gas prior to its entering the dryer or even in the dryer itself.
  • the effects can be general if vapours are added to the drying gas prior to entering the dryer or localized if vapours with or without gas are added inside the dryer.
  • the content of one or more solvents in the liquid feed may be adjusted.
  • the selected dew point may conveniently be adjusted prior to the addition of an optional auxiliary gas.
  • the auxiliary gas may be added in some types of close-cycled system to compensate for the escape of gas and evaporation of volatile compounds.
  • the predetermined dew point may be decreased slightly, however, usually not severely.
  • the drying gas being supplied to the drying chamber comprises one or more solvent vapours be- ing provided with a predetermined dew point before an optional auxiliary gas is added.
  • the drying gas being supplied to the drying chamber comprises one or more solvent vapours be- ing provided with a predetermined dew point before an optional auxiliary gas is added.
  • two or more solvent vapours are used, said two or more solvent vapours being provided with a common dew point prior to the optional addition of the auxiliary gas.
  • the common dew point is provided by process- ing the drying gas in a condenser.
  • the condensing may take place in one or more stages.
  • the condenser is preceded by, combined with or replaced by a scrubber capable of adjusting the concentration of one or more solvent vapours.
  • the scrubbing may happen in one or more stages at controlled temperature conditions.
  • the scrubber may be a dry scrubber or a wet scrubber, the latter optionally operating in a condensing scrubber mode.
  • the dew point of the sol- vent vapour is 20°C or more, preferably 30 °C or more. In another embodiment the dew point of the solvent vapour is 40°C or more, preferably 50 °C or more. Operating at a high relative humidity makes it possible to extensively affect the processing of particles. In preferred aspect water is used as the solvent vapour to form the above mentioned rela- tive humidities.
  • the drying is delayed by increasing the solvent vapour content to allow chosen properties of the particles to be developed.
  • the rate of evaporation of said volatile component can be reduced, whereby evaporation of other volatile components in the feed may be facilitated.
  • the liquid temperature can be raised during the evaporation, whereby liquid phase reactions can be accelerated and potentially be completed before the liquid is evaporated.
  • particle mor- phology can be influenced. For example, the powder and particle density can be affected as well as the ratio between crystalline and amorphous material in the final product.
  • one is water.
  • a second solvent which is miscible with water, is also present.
  • the solvent which is miscible with water
  • Further water miscible solvents include acetone, diethylether, ethyl acetate, acetonitrile and methylethylketone.
  • none of the solvent vapours are aqueous.
  • one or more of said non-aqueous solvents is selected among perfluorocarbons, dichloromethane, chloroform, ether, ethyl acetate, methyl-tert-butyl ether, hexane, heptane, n-dodecane, m-xylene, isopentene isooctane, tetrahydrofuran, dimethyl sulfoxide, dimethylformamide, toluene, glacial acetic acid, and acetonitrile.
  • the drying gas being sup- plied to the chamber comprises two or more solvent vapours having different dew points.
  • a dew point is selected to promote the evaporation of a solvent component from the particles being formed or to suppress the evaporation of a solvent component from the particles being formed.
  • a dew point of a solvent vapour is selected to suppress the evaporation of a solvent component from the particles being formed.
  • the liquid feed which is introduced into the drying chamber, comprises a solution or suspension of biomolecules, such as proteins, monoclonal antibodies, vaccines, synthetic peptides or oligonucleotides, in an organic solvent such as acetonitrile or acetone, and furthermore water in an amount of 1-10% (vol/vol), preferably 3% (vol/vol), is added to the liquid feed.
  • biomolecules such as proteins, monoclonal antibodies, vaccines, synthetic peptides or oligonucleotides
  • organic solvent such as acetonitrile or acetone
  • water in an amount of 1-10% (vol/vol), preferably 3% (vol/vol) is added to the liquid feed.
  • the proteins may be industrial enzymes like
  • Figure 1 shows an embodiment of a plant for carrying out the process according to the invention.
  • 1 is feed for feeding to the chamber 2 of a spray dryer; 3 is a cyclone for recovering a main powder fraction 4 from the product stream leaving the spray dryer; 5 is a bag filter for recovering fines 6 from the exhaust gases received from the cyclone; 7 and 15 are high efficiency particulate air (HEPA) filters for re- moving a substantial part of residual airborne particles; 8 is a condenser; 9 is discharged condensate of solvent; 10 is a scrubber, 14 is a heaters; 11 is an inlet and/or discharge for auxiliary gas; 13 is a fan; 16 is a pipe for addition of solvent and/or solvent vapour to the stream of drying gas prior to its entrance into the chamber of the spray dryer; 17 is a pipe for addition of solvent and/or solvent vapour/gas to a specific location within the spray dryer; 18 is a pipe for supplying additional drying gas.
  • HEPA high efficiency particulate air
  • a feed stream 1 to be processed is received in the drying chamber 2 of a closed cycle spray dryer using an inert drying gas.
  • the stream of drying gas is passed through the HEPA filter 7 such as to arrive at the condenser 8, from which condensed solvent 9 may be removed.
  • the gas stream is treated in the scrubber 10, wherein its content of solvents is adjusted by selective removal or addition of gas stream components.
  • the scrubber 10 may be posi- tioned prior or the condenser 8.
  • a first solvent originates from the feed material, while a second solvent is added as a co-solvent to promote evaporation of the first solvent.
  • the scrubber is operated such as to selectively trap vapour of the first solvent.
  • the pressure in the cyclic drying system is maintained by additional supply of the auxiliary gas at the inlet 11 as required.
  • additional quantities of the second solvent is added to the stream of drying gas prior to its entrance into the chamber of the spray dryer, aiming for a pre- established optimum dew point, at which the net effect of the second solvent as an aid-solvent to promote the evaporation of the first solvent is most pronounced.
  • the steps of condensing and scrubbing might have been interchanged by making use of a wet scrubber operating in a condensing scrubber mode, or the scrubber 12 might have been interposed in an alternative position between the HEPA filter 7 and the condenser 8.
  • drying gas would have been supplied to the plant at an immediately upstream position relative to the condenser 8 and possibly the scrubber 12 in said alternative position, whereas gas exhaust from the plant would take place at a position just downstream the HEPA filter 7.
  • the drying system might have been run with a feed and drying gas presenting a single predominant solvent.
  • the dew point of the solvent vapour is managed by condensation and/or scrubbing and/or addition of further solvent in order to attain optimum properties of the resultant particles, e.g. with regard to density, morphology and residual solvent content.
  • the addition of further solvent might happen through the pipe 17, so that the solvent vapour is released directly into the spraying chamber, possibly to a confined area around the spray nozzle with a view to enhanced suppression of drying in this zone.
  • the choice of an appropriate dew point and solvent is informed by preceding drying trials, e.g.
  • the process for the preparation of spray dried particles comprises the steps of:
  • the solvent mixture comprises a main solvent and a co- solvent.
  • Embodiments, wherein a second solvent is added as a co- solvent to promote evaporation of a first solvent have important application in the processing of biomolecules, e.g. for biopharmaceutical applications. For instance, when spray drying a feed of proteins in acetone with a small amount of water, it is possible to preferentially remove the more volatile organic solvents by varying the amount of water in the feed and processing at low temperature, e.g. with an outlet temperature in the range of -10 to 40 °C. For other products it may be possible to operate in the range of -10 to 80°C, especially when the biomolecules is less sensitive.
  • polar organic solvents can bind to the same hydrophilic sites on the protein as the polar water molecules, and once they are bound they cannot be removed.
  • adding water as a co-solvent to the feed allows the organic solvents to be driven off faster as they are more volatile, while the water molecules protect the hydrophilic sites from having an organic solvent mole- cule bind to them.
  • the residual contents of water and organic solvent in the powders may be tuned by varying both the relative amount of water in the feed suspension and the outlet temperature of the spray drying process.
  • the process may e.g. be relevant for solutions of recombinant proteins, monoclonal antibodies, vaccines, synthetic peptides and oligonucleotides in organic solvents such as ace- tonitrile or acetone which are both polar solvents and miscible with water, which is an important point in this context.
  • organic solvents such as ace- tonitrile or acetone which are both polar solvents and miscible with water, which is an important point in this context.
  • Conventional spray drying of these temperature-sensitive macromolecules typically results in 2 or 3% residual solvent in the powders, until a sufficiently high outlet temperature of 70°C or higher is reached, at which temperature the molecules are typically denatured . This means that the acceptable limit for residual organic solvent cannot be met using conventional spray drying, because the organic solvents bind to the hydrophilic sites on the mole- cule, and increasing heat does not drive off additional solvent.
  • a great deal of linear peptide synthesis is either carried out in organic solvents or may include a final rinsing step with an organic solvent cocktail, which may then be lyophilized.
  • an organic solvent cocktail which may then be lyophilized.
  • a co-solvent such as water
  • the invention may be applied on microorganisms, which is se- lected from the group comprising bacteria, virus, yeast, fungus and algae to obtain dried particles including these microorganisms.
  • the present invention is also useful in the formulation of a solid dispersion comprising a hydrophilic polymer and a bioactive compound having low aqueous solubility and dissolution rate.
  • the solid dispersion improves the solubility and dissolution rate of the bioactive compound having low aqueous solubility and dissolution rate, such as BCS Class II or Class IV drug compounds.
  • BCS Biopharmaceutics Classification System
  • BCS restricts the prediction us- ing the parameters solubility (high/low) and intestinal permeability (high/low).
  • BCS Class II compounds have high permeability and low solubility
  • BCS Class IV compounds have low permeability and low solubility.
  • the bioactive compound is dissolved or suspended in a liquid feed together with a hydrophilic polymer, which includes polymers well known in pharmaceutical compositions e.g. a polymer selected among the group consisting of hydroxy- propyl methylcellulose (HPMC), hydroxypropylmethylcellulose acetate succinate (HPMCAS), polyvinylpyrrolidone (PVP), and vinylpyrrolidone- vinyl acetate copolymers.
  • a hydrophilic polymer which includes polymers well known in pharmaceutical compositions e.g. a polymer selected among the group consisting of hydroxy- propyl methylcellulose (HPMC), hydroxypropylmethylcellulose acetate succinate (HPMCAS), polyvinylpyrrolidone (PVP), and vinylpyrrolidone- vinyl acetate copolymers.
  • HPMC hydroxy- propyl methylcellulose
  • HPMCAS hydroxypropylmethylcellulose acetate succinate
  • PVP polyvinylpyrrolidone
  • the spray dried particles resulting from any of the processes disclosed herein may be post-processed, including post-drying, post- cooling, post-crystallisating, and any combination thereof.
  • the post- drying may be performed in a fluid bed.
  • the particles produced according to the process described above may be useful within various industries including the pharmaceutical, food, diary, and chemical industry.
  • the presence of certain second solvents is observed to promote the drying of certain first solvents. Accordingly, the residual level of the first solvent in the dried product is lower if a suitable second solvent is present during otherwise identical drying conditions. However, prema- ture drying off of the solvent meant to aid the drying may prevent the desired result. If the vapour composition in the drying gas is optimized (most frequently impossible in traditional dehumidifiers and condensers) to retain a specific level of second aid-solvent(s) in the product, while at the same time good conditions are provided for the evaporation of the more persistent first solvent(s), optimum results are achieved.
  • Bovine serum albumine or salmon calcitonin in a solution of acetone or acetonitrile together with water in an amount of 3 % (vol/vol) is fed into a drying chamber. Due to this procedure, a sufficiently low level of organic solvent in the final product can be attained while still operating at a modest temperature, which is harmless to the protein in question. In addition, a fully acceptable residual water content in the range of 1-4% is also accomplished.

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  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Drying Of Solid Materials (AREA)

Abstract

La présente invention a pour objet un procédé de préparation de particules séchées par pulvérisation, ledit procédé comprenant les étapes suivantes : la pulvérisation dans une chambre d'une charge de liquide comprenant un ou plusieurs solvants et l'apport d'un gaz de séchage dans la chambre avec une ou plusieurs vapeurs de solvants présentant un point de saturation choisi pour procurer une propriété souhaitée aux particules séchées par pulvérisation.
PCT/DK2011/050209 2010-06-11 2011-06-10 Séchage contrôlé de l'humidité WO2011154014A1 (fr)

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DKPA201000517 2010-06-11
DKPA201000517 2010-06-11

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10463621B2 (en) 2014-03-31 2019-11-05 Hovione Holding Limited Spray drying process for production of powders with enhanced properties
CN114466686A (zh) * 2019-07-02 2022-05-10 豪夫迈·罗氏有限公司 用于制备具有受控湿度的高亲水性类型产物的方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5985248A (en) * 1996-12-31 1999-11-16 Inhale Therapeutic Systems Processes for spray drying solutions of hydrophobic drugs and compositions thereof
WO2002085326A2 (fr) * 2001-04-18 2002-10-31 Advanced Inhalation Research, Inc. Regulation d'humidite de procede afin de produire des particules poreuses de grandes dimensions
US20030163931A1 (en) * 2002-02-01 2003-09-04 Beyerinck Ronald A. Method for making homogeneous spray-dried soild amorphous drug dispersions utilizing modified spray-drying apparatus
WO2003079993A2 (fr) * 2002-03-20 2003-10-02 Advanced Inhalation Research, Inc. Preparations d'hormone de croissance humaine (hch) destinees a etre administrees par voie pulmonaire
WO2005011636A2 (fr) * 2003-08-04 2005-02-10 Pfizer Products Inc. Procedes de sechage par atomisation pour former des dispersions amorphes solides de medicaments et de polymeres
US20070172430A1 (en) * 2006-01-20 2007-07-26 Nastech Pharmaceutical Company Inc. Dry powder compositions for rna influenza therapeutics
EP2172190A1 (fr) * 2008-10-02 2010-04-07 Laboratorios Liconsa, S.A. Particules inhalables comprenant du tiotropium

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5985248A (en) * 1996-12-31 1999-11-16 Inhale Therapeutic Systems Processes for spray drying solutions of hydrophobic drugs and compositions thereof
WO2002085326A2 (fr) * 2001-04-18 2002-10-31 Advanced Inhalation Research, Inc. Regulation d'humidite de procede afin de produire des particules poreuses de grandes dimensions
US7469488B2 (en) 2001-04-18 2008-12-30 Alkermes, Inc. Control of process humidity to produce large, porous particles
US20030163931A1 (en) * 2002-02-01 2003-09-04 Beyerinck Ronald A. Method for making homogeneous spray-dried soild amorphous drug dispersions utilizing modified spray-drying apparatus
WO2003079993A2 (fr) * 2002-03-20 2003-10-02 Advanced Inhalation Research, Inc. Preparations d'hormone de croissance humaine (hch) destinees a etre administrees par voie pulmonaire
WO2005011636A2 (fr) * 2003-08-04 2005-02-10 Pfizer Products Inc. Procedes de sechage par atomisation pour former des dispersions amorphes solides de medicaments et de polymeres
US20070172430A1 (en) * 2006-01-20 2007-07-26 Nastech Pharmaceutical Company Inc. Dry powder compositions for rna influenza therapeutics
EP2172190A1 (fr) * 2008-10-02 2010-04-07 Laboratorios Liconsa, S.A. Particules inhalables comprenant du tiotropium

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Title
MAA YF ET AL: "Effect of spray drying and subsequent processing conditions on residual moisture content and physical/biochemical stability of protein inhalation powders", PHARMACEUTICAL RESEARCH, KLUWER ACADEMIC PUBLISHERS, NEW YORK, NY, US, vol. 15, no. 5, 1 May 1998 (1998-05-01), pages 768 - 775, XP002114088, ISSN: 0724-8741, DOI: 10.1023/A:1011983322594 *
VEHRING ET AL: "Particle formation in spray drying", JOURNAL OF AEROSOL SCIENCE, PERGAMON, vol. 38, no. 7, 1 July 2007 (2007-07-01), pages 728 - 746, XP022167042, ISSN: 0021-8502, DOI: 10.1016/J.JAEROSCI.2007.04.005 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10463621B2 (en) 2014-03-31 2019-11-05 Hovione Holding Limited Spray drying process for production of powders with enhanced properties
US10918603B2 (en) 2014-03-31 2021-02-16 Hovione Holding Limited Spray drying process for production of powders with enhanced properties
CN114466686A (zh) * 2019-07-02 2022-05-10 豪夫迈·罗氏有限公司 用于制备具有受控湿度的高亲水性类型产物的方法

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