AAPS PharmSci

, Volume 5, Issue 4, pp 77–89 | Cite as

Properties of microcrystalline cellulose and powder cellulose after extrusion/spheronization as studied by fourier transform Raman spectroscopy and environmental scanning electron microscopy

  • Petra M. Fechner
  • Siegfried Wartewig
  • Manfred Füting
  • Andreas Heilmann
  • Reinhard H. H. Neubert
  • Peter Kleinebudde


In this study, the effect of powder cellulose (PC) and 2 types of microcrystalline cellulose (MCC 101 and MCC 301) on pellet properties produced by an extrusion/spheronization process was investigated. The different investigated types of cellulose displayed different behavior during the extrusion/spheronization process. Pure PC was unsuitable for extrusion, because too much water was required and the added water was partly squeezed during the extrusion process. In contrast, MCC 101 and MCC 301 were extrudable at a wide range of water content, but the quality of the resulting products varied. In the extrusion/spheronization process, MCC 101 was the best substance, with easy handling and acceptable product properties. The properties of the extrudates and pellets were determined by Fourier transform (FT) Raman spectroscopy and environmental scanning electron microscopy (ESEM). FT-Raman spectroscopy was able to distinguish between the original substances and also between the wet and dried extrudates. The particle sizes of the raw material and of the extrudates were determined by ESEM without additional preparation. For MCC, the size of the resulting particles within the extrudate or pellet was smaller. However, in the extrudates of PC, changes in particle size could not be observed.


powder cellulose microcrystalline cellulose pellet Raman spectroscopy environmental scanning electron microscopy extrusion/spheronization 


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  1. 1.
    Wallace JW. Cellulose derivatives and natural products utilized in pharmaceutics. In: Swarbrick J, Boylan JC, eds. Encyclopedia of Pharmaceutical Technology. New York, NY: Marcel Dekker; 1991;319–337.Google Scholar
  2. 2.
    Newton JM. Extrusion and extruders. In: Swarbrick J, Boylan JC, eds. Encyclopedia of Pharmaceutical Technology. New York, NY: Marcel Dekker; 2002;1220–1236.Google Scholar
  3. 3.
    Edwards HGM, Farwell DW, Williams AC. FT-Raman spectrum of cotton: a polymeric biomolecular analysis. Spectrochim Acta A Mol Biomol Spectrosc. 1994;50A(4):807–811.CrossRefGoogle Scholar
  4. 4.
    Langkilde FW, Svantesson A. Identification of celluloses with Fourier-Transform (FT) mid-infrared, FT-Raman and near-infrared spectrometry. J Pharm Biomed Anal. 1995;13(4/5):409–414.PubMedCrossRefGoogle Scholar
  5. 5.
    Hopfe J, Füting M. Fundamentals and applications of environmental scanning electron microscopy. In: Wetzig K, Schulze D, eds. In Situ Scanning Electron Microscopy in Materials Research. Berlin, Germany: Akademie Verlag GmbH; 1995:219–240.Google Scholar
  6. 6.
    Baert L, Remon JP, Knight P, Newton JM. A comparison between the extrusion forces and sphere quality of a gravity feed extruder and a ram extruder. Int J Pharm. 1992;86:187–192.CrossRefGoogle Scholar
  7. 7.
    Dietrich R. Food technology transfers to pellet production. Manuf Chemist. 1989;60; Aug: 29–33.Google Scholar
  8. 8.
    Harrison PJ, Newton JM, Rowe RC. Flow defects in wet powder mass extrusion. J Pharm Pharmacol. 1985;37:81–83.PubMedCrossRefGoogle Scholar
  9. 9.
    Kleinebudde P, Lindner H. Experiments with an instrumented twin-screw extruder using a single-step granulation/extrusion process. Int J Pharm. 1994;94:49–58.CrossRefGoogle Scholar
  10. 10.
    Fielden KE, Newton JM, O Brien P, Rowe RC. Thermal studies on the interaction of water and microcrystalline cellulose. J Pharm Pharmacol. 1988;40:674–678.PubMedCrossRefGoogle Scholar
  11. 11.
    Kleinebudde P. The crystallite-gel-model for microcrystalline cellulose in wet-granulation, extrusion, and spheronization. Pharm Res. 1997;14(6):804–809.PubMedCrossRefGoogle Scholar
  12. 12.
    Kleinebudde P, Jumaa M, Saleh FE. Influence of degree of polymerization on behavior of cellulose during homogenization and extrusion/spheronization. AAPS PharmSci. 2000;2(2) article 21.Google Scholar
  13. 13.
    Jumaa M, Saleh FE, Hassan I, Müller BW, Kleinebudde P. Influence of cellulose type on the properties of extruded pellets, I: physicochemical characterisation of the cellulose types after homogenisation. Colloid Polym Sci. 2000;278(7):597–607.CrossRefGoogle Scholar
  14. 14.
    Heng PWS, Koo OMY. A study of the effects of the physical characteristics of microcrystalline cellulose on performance in extrusion spheronization. Pharm Res. 2001;18(4):480–487.PubMedCrossRefGoogle Scholar
  15. 15.
    Kristensen J, Schaefer T, Kleinebudde P. Direct pelletization in a rotary processor controlled by torque measurements, II: effect of changes in the content of microcrystalline cellulose. AAPS PharmSci. 2000;2(3) article 24.Google Scholar
  16. 16.
    MacRitchie KA, Newton JM, Rowe RC. The evaluation of the rheological properties of lactose/microcrystalline cellulose and water mixtures by controlled stress rheometry and the relationship to the production of spherical pellets by extrusion/spheronization. Eur J Pharm Sci. 2002;17:43–50.PubMedCrossRefGoogle Scholar
  17. 17.
    Law MFL, Deasy PB. Use of hydrophilic polymers with microcrystalline cellulose to improve extrusion-spheronization. Eur J Pharm Biopharm. 1998;45:57–65.PubMedCrossRefGoogle Scholar
  18. 18.
    Lindner H, Kleinebudde P. Use of powdered cellulose for the production of pellets by extrusion/spheronization. J Pharm Pharmacol. 1994;46:2–7.PubMedCrossRefGoogle Scholar
  19. 19.
    Saleh FE, Jumaa M, Hassan I, Kleinebudde P. Influence of cellulose type on the properties of extruded pellets. II: production and properties of pellets. STP Pharm Sci. 2000;10(5):379–385.Google Scholar
  20. 20.
    Koo OMY, Heng PWS. The influence of microcrystalline cellulose grade on shape and shape distributions of pellets produced by extrusion-spheronization. Chem Pharm Bull. 2001;49(11):1383–1387.PubMedCrossRefGoogle Scholar
  21. 21.
    Blackwell J, Vasko PD, Koenig JL. Infrared and Raman spectra of the cellulose from the cell wall of Valonia ventricosa. J Appl Phys. 1970;41:4375–4379.CrossRefGoogle Scholar

Copyright information

© American Association of Pharmaceutical Scientists 2003

Authors and Affiliations

  • Petra M. Fechner
    • 1
  • Siegfried Wartewig
    • 2
  • Manfred Füting
    • 3
  • Andreas Heilmann
    • 3
  • Reinhard H. H. Neubert
    • 1
  • Peter Kleinebudde
    • 4
  1. 1.Institute of Pharmaceutics and BiopharmaceuticsMartin Luther University Halle-WittenbergHalleGermany
  2. 2.Institute of Applied DermatopharmacyMartin Luther University Halle-WittenbergHalleGermany
  3. 3.Fraunhofer Institute for Mechanics of MaterialsHalleGermany
  4. 4.Institute of Pharmaceutical TechnologyHeinrich Heine University DüsseldorfDüsseldorfGermany

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