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PRODUCTION OF NANO PARTICLES USING SUPERCRITICAL CO2. By Satya Chaitanya Class 702 - Modules in nano pharmaceuticals Dr.Rajesh Dave. What is S uper C ritical F luid? A fluid is compressed beyond its Pc and heated beyond its Tc. Why we choose CO2:

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production of nano particles using supercritical co2

PRODUCTION OF NANO PARTICLES USING SUPERCRITICAL CO2

By

Satya Chaitanya

Class

702 - Modules in nano pharmaceuticals

Dr.Rajesh Dave

slide2
What is Super Critical Fluid?
  • A fluid is compressed beyond its Pc and heated beyond its Tc.

Why we choose CO2:

  • nonflammable, nontoxic, Low dielectric constant, inexpensive, mild Tc.

Solubility

  • Non polar or light molecules easily dissolve in CO2.
  • Heavy molecules have a very poor solubility.
slide3
Three important factors that govern drug solubility
  • vapor pressure. f (T)
  • CO2 interaction.
  • Density of CO2. f (P,T).

The solubility can be correlated by using the equation

An empirical expression for density is given below

slide4
The most studied SF-based micronization techniques are
  • Rapid Expansion of Supercritical Solutions (RESS)
  • Supercritical Anti Solvent precipitation (SAS)
  • Supercritical fluids Assisted Atomization (SAA)
  • Particles generation from Gas Saturated Solutions (PGSS)
  • Supercritical Carbon dioxide Assisted Nebulization (CAN-BD)

with a Bubble Dryer.

slide7
RESS with solid co-solvent for nano particle formation

RESS-SC

RESS-SC is a modification of

RESS process and overcomes the

limitations of RESS.

Setup is divided into 3 parts

Pre extraction chamber (section I).

Extraction chamber (section II).

Expansion chamber (section III).

slide8
The choice of a proper SC is the key for successful RESS-SC.
  • Requirements for the selection of the SC are
  • Good solubility in supercritical CO2.
  • Solid at nozzle exit condition (5–30 °C).
  • Good vapor pressure for easy removal by sublimation.
  • Nonreactive with drugs or CO2.
  • Inexpensive.
slide9
Magnified view of the RESS nozzle. (B) Schematic of

RESS–SC process. Circles-drug particles, Stars-SC particles.

slide12
SAS with Enhanced Mass transfer (SAS-EM) process for nanoparticle formation

I, inline filter; U, ultrasonic processor; P, pump for drug solution; R, precipitation chamber; SCF pump, supply of supercritical CO2; G, pressure gauge; C, heating coil with temperature controller.

slide13
At higher power supply to the ultrasound transducer, narrower and shorter needle shaped crystals were obtained.

size of the precipitated GF nanoparticles Volume of long needle shaped GF crystals obtained

versus power supply to the ultrasound transducer, for power 75 W.

slide14
SEM micrographs showing the change in the morphologies of GF particles obtained from experiments conducted at different

values of power supply using DCM as solvent. (a) No power supply, (b) 60 W power supply, (c) 90 W power supply, (d) 120 W

power supply, (e) 150 W power supply, (f) 180 W power supply. Magnification is ×1000

slide17
Two atomization processes take place
  • Primary droplets at the outlet of the injector (pneumatic atomization) are further divided in
  • Secondary droplets due to SC-CO2 expansion from the inside of the primary ones (decompressive atomization).

Pneumatic atomization Decompressive atomization

Amorphous or crystalline particles have been produced, depending on the process temperatures and the chemical characteristics of the solid solute.

slide18

Experiments were performed varying

HMR1031 concentration (50 to 150 mg/ml) in the methanol solution.

SEM observations revealed that SAA micronized particles are spherical whereas the jet-milled particles are irregular in shape.

Particles from SAA

Particles from Jet-mill

slide19
PSDs of the SAA micronized drug were measured by laser diffraction.
  • curves of HMR1031 produced by SAA from HMR1031 concentrations
slide20
Griseofulvin nano particles
  • The particles obtained are spherical and noncoalescing.
can bd process carbon dioxide assisted nebulization with a bubble dryer schematic of bubble dryer
CAN-BD Process(Carbon Dioxide Assisted Nebulization with a bubble Dryer)Schematic of Bubble Dryer
slide26
References
  • Thakur R, Gupta RB. Rapid expansion of supercritical solution with solid cosolvent (RESS-SC) process: formation of griseofulvin nanoparticles. Ind Eng Chem Res 2005. In press.
  • Chattopadhyay P, Gupta RB. Production of griseofulvin nanoparticles using supercritical CO2 antisolvent with enhanced mass transfer. Int J Pharm 2001; 228(1–2):19–31.
  • Production of griseofulvin nanoparticles using supercritical CO2 anti solvent with enhanced mass transfer * Pratibhash cattopadhyay, Ram B. Gupta AL 36839 -5127, USA Received 19 February 2001; received in revised form 3 July 2001; accepted 5 July 2001.
  • Supercritical Assisted Atomization: A Novel Technology for Microparticles Preparation of an Asthma-controlling Drug *Giovanna Della Porta, Carlo De Vittori, and Ernesto Reverchon
slide27
Other references
  • Coffey MP, Krukonis VJ. Supercritical Fluid Nucleation. An Improved Ultrafine Particle Formation Process. Phasex Corp.Final Report to NSF, 1988, Contr. ISI 8660823.
  • Pathak P, Meziani MJ, Desai T, Sun Y-P. Nanosizing drug particles in supercritical fluid processing. J Am Chem Soc 2004;126:10,842.
  • Turk M, Hils P, Helfgen B, Schaber K, Martin H-J, Wahl MA.Micronization of pharmaceutical substances by the rapidexpansion of supercritical solutions (RESS): a promisingmethod to improve the bioavailability of poorly soluble pharmaceutical agent. J Supercrit Fluids 2002; 22:75.
  • 20. Mohamed RS, Halverson DS, Debenedetti PG, Prud’homme RK.Solids formation after the expansion of supercritical mixtures.In: Johnston KP, Penninger JML, eds. Supercritical Fluid Science and Technology. Washington, DC: ACS Symposium Series 406, 1989:355–378.