Characterization of microspheres

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this presentation includes various evaluation tests of Microspheres

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Characterization of microspheres

  1. 1. Characterization of Microspheres By Mr. Thoke Sagar B.
  2. 2. Characterization Properties Of Microspheres1] Particle size analysis2] Scanning electron microscopy (SEM) study3] Flow properties4] Thermal analysis5] Determination of percentage yield6] Drug content7] Determination of drug loading2
  3. 3. 8] Incorporation efficiency of microspheres9] Determination of solubility10] Dissolution studies of microspheres 3
  4. 4. 1] Particle size analysis Particle size of recrystallized sample, pure samples, spays driedmicrospheres were determined by microscopic method usingcalibrated ocular micrometer. A microscopical image analysis technique for determination ofparticle size was applied. The morphology and particle sizes weredetermined in a Digital microscope equipped with a 1/3”CCDcamera imaging accessory The microspheres were dispersed on a microscope slide. Amicroscopical field was scanned by video camera. The images ofthe scanned field are analyzed by the softwar. 4
  5. 5. 2] Scanning electron microscopy (SEM) study The morphology of microspheres was examined by scanningelection microscopy. A small amount of powder was spread on analuminum stub, which was placed latter gold sputtering in san SEMchamber. Photographs were taken at an acceleration voltages of 20 KVelectron beam. Obtained photograph to identify and confirmspherical nature and Surface topography of the crystals. 5
  6. 6. 3] Flow properties Flow properties of the microspheres were evaluated bydetermining the angle of repose and the compressibility index. a) The angle of repose of microsphere and commercialcrystals was measured by fixed funnel method. Static angle of repose was measured according to the fixedfunnel and free standing cone method of Banker and Anderson. A funnel with the end of the stem cut perpendicular to the axisof symmetry is secured with its tip at a given height (1 cm), H,above graph paper placed on a flat horizontal surface. Themicrospheres were carefully poured through the funnel until theapex of the conical pile so formed just reached the tip of thefunnel. 6
  7. 7. Thus, the R being the radius of the base of the microspheresconical pile: . tan θ = H/ R or θ = tan-1 (H/ R) where θ = the angle of repose 7
  8. 8. b) Compressibility index (I): Carr’s index was determined from powder volumes at theinitial stage and after 1250 tappings to constant volume. Compressibility index (I) values of the microspheres weredetermined by measuring the initial volume (V0) and the finalvolume (V) after subjecting to 100 tapping in a graduatedmeasuring cylinder using the equation. I = [1- (V/V0)] x 100 Apparent particle densities of microsphere were measuredusing a Pycnometer. 8
  9. 9. 4] Thermal analysis Differential scanning calorimeter (DSC) DSC study was carried out to detect possible polymorphictransition during the crystallization process. DSC measurementswere performed on differential scanning calorimeter (DSC DuPont9900) with a thermal analyzer. Differential scanning calorimetry (DSC) was performed onketoprofen and ketoprofen loaded microspheres. DSCmeasurement were done on a Mettler Toledo DSC 822c C/ minover a temperature range of 30 to 30000 C under an inertatmosphere flushed with nitrogen at a rate of 20 ml/min. 9
  10. 10. 5] Determination of percentage yield The yield of microspheres was determined by the formula, %Yield= Total Weight of Microspheres ------------------------------------------ x 100 Total Weight of Raw Material The percentage yield of each formulation was determinedaccording to the total recoverable finalweight of microsphere andthe total original weight of Indomethacin. 10
  11. 11. 6] Drug content Microspheres in a particular quantity were dissolve in a solventand at specified λmax of drug . The drug content of Microspheres isestimated. Microspheres (50 mg) were triturated with 10 ml of water.Allowed to stand for 10 min withoccasional swirling and methanolwas added to produce 100 ml. After suitable dilution, samplesweremeasured at particular λmax value of drug. Drug content wasdetermined from standard plot. 11
  12. 12. 7] Determination of drug loadingThe drug loading was determined by UV‐Visible spectrophotometer.The microspheres were stirred with 100 ml particular solution asdissolution media (pH 7.40 phasphatebuffer )for 2hr. The drugconcentration will be determin at particular λmax value of drug aftersuitable dilution. The readings were taken in triplicate.Drug loading (%) = M actual ------------------------------ x 100 Weighed quantity of powder of microspheres 12
  13. 13. 8] Incorporation efficiency of microspheresIncorporation efficiency (%) = M actual ---------------------- x 100 M theoreticalWhere,M actual is the actual drug content in weighed quantity of powderof microspheres &M theoretical is the theoretical amount of drug in microspherescalculated from the quantity added in the fabrication process. 13
  14. 14. 9] Determination of solubilityThe solubility of particular drug microspheres in specific solutionas microspheres or microcapsule to be soluble in that particularenvironment (water and pH 7.4 phosphate buffer) was determinedby taking excess quantity of microspheres in 50 ml to screw‐cappedglass vials filled with water. The vials were shaken for two hours onmechanical shaker. The solution was filtered through Whatmannfilter paper No.1 and drug concentration wasbe determined atparticular λmax value of drug. 14
  15. 15. 10] Dissolution studies of microspheresThe dissolution of microspheres is determined by using USPdissolution apparatus XXIV Type II. Dissolution medium was900 ml 7.4 Phosphate buffer. The amount of dissolved drug wasdetermined using UV spectrophotometric method at specifiedλmax of particular drug. The readings were taken in triplicate. 15
  16. 16. References1] S. B. Gholap,International Journal of Pharmaceutical Sciences Review and Research, Issue: 1, Volume 1, March – April 2010; Article 015,Page no.- 782] MUDIT DIXIT, International Journal of Drug Formulation & Research,ISSN: 2229-5054, Volume 2 (1),Jan-Feb.2011, Page no.- 142-1433] Deore B.V.,International Journal of ChemTech Research,ISSN: 0974-4290, Volume 1, No.3, July-Sept 2009,page no.-635-636.4] ASHWINI G KINI, International Journal of Pharmacy andPharmaceutical Sciences,ISSN: 0975-1491,Volume 3, Suppl 2,2011, Page no- 232.16
  17. 17. Contact on:- Mob. No.- +918275584727  Email ID:-  thokesagar7@gmail.com  thokesagar@yahoo.com Thank you...17

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