Journal of Pharmaceutical Innovation

, Volume 4, Issue 4, pp 187–197 | Cite as

Near-infrared Spectroscopy for the In-line Characterization of Powder Voiding Part I: Development of the Methodology

  • Jorge Ropero
  • Lauren Beach
  • Manel Alcalà
  • Raizza Rentas
  • Rajesh N. Davé
  • Rodolfo J. RomañachEmail author
Research Article


In-line near-infrared spectroscopy (NIR) spectra were acquired and analyzed to assess the relationship between physical and chemical properties of voiding powders and their spectral changes. NIR spectra were obtained for powders voiding from a conical glass funnel while the powder flow was recorded with a digital camera. Two different approaches using in-line NIR spectra were developed to measure the flow interruptions in the powder voiding process. The first approach uses the noise in the spectra and the second is based on the baseline changes. The new method was also used to evaluate the effects of humidity on the flow of microcrystalline cellulose samples and to evaluate the effect of mixing method on the flow properties of the blends obtained. The method described may be applied to other applications that involve powder flow, and the same spectra may be used to determine drug concentration.


Powder flow Near-infrared spectroscopy In-line monitoring Process analytical technology Quality by design 



Authors acknowledge the support of National Science Foundation (ERC research grant: EEC-0540855) for conducting this research work.

Supplementary material


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  1. 1.
    Schneider LCR, Sinka IC, Cocks ACF. Characterisation of the flow behaviour of pharmaceutical powders using a model die–shoe filling system. Powder Technol. 2007;173:59–71.CrossRefGoogle Scholar
  2. 2.
    Wang C, Hassanpour A, Ghadiri M. Characterisation of flowability of cohesive powders by testing small quantities of weak compacts. Particuology. 2008;6:282–5.CrossRefGoogle Scholar
  3. 3.
    Castellanos A, Valverde JM, Quintanilla MAS. The Sevilla powder tester: a tool for characterizing the physical properties of fine cohesive powders at very small consolidations. Kona. 2004;22:66–81.Google Scholar
  4. 4.
    Taylor MK, Ginsburg J, Hickey AJ, Gheyas F. Composite method to quantify powder flow as a screening method in early tablet or capsule formulation development. AAPS PharmSciTech. 2000;1(3):article 18.Google Scholar
  5. 5.
    Navaneethan CV, Missaghi S, Fassihi R. Application of powder rheometer to determine powder flow properties and lubrication efficiency of pharmaceutical particulate systems. AAPS PharmSciTech. 2005;06:E398–404.CrossRefGoogle Scholar
  6. 6.
    Thalberg K, Lindholm D, Axelsson A. Comparison of different flowability tests for powders for inhalation. Powder Technol. 2004;146:206–13.CrossRefGoogle Scholar
  7. 7.
    Benedetti C, Abatzoglou N, Simard JS, McDermott L, Leonard G, Cartilier L. Cohesive, multicomponent, dense powder flow characterization by NIR. Int J Pharm. 2007;336:292–301.CrossRefPubMedGoogle Scholar
  8. 8.
    Hancock B, Vukovinsky K, Brolley B, Grimsey I, Hedden D, Olsofsky A, et al. Development of a robust procedure for assessing powder flow using a commercial avalanche testing instrument. J Pharm Biomed Anal. 2004;35:979–90.CrossRefPubMedGoogle Scholar
  9. 9.
    Barajas M, Rodriguez A, Vargas W, Conde C, Ropero J, Figueroa J, et al. Near-infrared spectroscopic method for real-time monitoring of pharmaceutical powders during voiding. Appl Spectrosc. 2007;65:490–6.CrossRefGoogle Scholar
  10. 10.
    Serway RA, Beichner RJ. Physics for scientists and engineers. Kentucky: Thomson Learning; 2000. p. 22–57.Google Scholar
  11. 11.
    Næs T, Isaksson T, Fearn T, Davies T. A user-friendly guide to multivariate calibration and classification. 1st ed. Chichester: NIR Publications; 2002.Google Scholar
  12. 12.
    Isaksson T, Griffiths P. Optimal absorbance for transmission or reflection spectra measured under conditions of constant detector noise in the presence of stray radiation. Appl Spectrosc. 2002;56:916–9.CrossRefGoogle Scholar
  13. 13.
    Blanco M, Alcala M. Content uniformity and tablet hardness testing of intact pharmaceutical tablets by near infrared spectroscopy a contribution to process analytical technologies. Anal Chim Acta. 2006;557:353–9.CrossRefGoogle Scholar

Copyright information

© International Society for Pharmaceutical Engineering 2009

Authors and Affiliations

  • Jorge Ropero
    • 1
  • Lauren Beach
    • 2
  • Manel Alcalà
    • 3
  • Raizza Rentas
    • 1
  • Rajesh N. Davé
    • 2
  • Rodolfo J. Romañach
    • 1
    Email author
  1. 1.Department of ChemistryUniversity of Puerto RicoMayagüezPuerto Rico
  2. 2.Department of Chemical EngineeringNew Jersey Institute of TechnologyNewarkUSA
  3. 3.Grup de Quimiometria Aplicada, Departament de Química (U. Analítica), Facultat de CiènciesUniversitat Autònoma de BarcelonaBellaterraSpain

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