Advertisement

AAPS PharmSciTech

, Volume 6, Issue 2, pp E262–E272 | Cite as

Process analytical technology case study part I: Feasibility studies for quantitative near-infrared method development

  • Robert P. Cogdill
  • Carl A. Anderson
  • Miriam Delgado-Lopez
  • David Molseed
  • Robert Chisholm
  • Raymond Bolton
  • Thorsten Herkert
  • Ali M. Afnán
  • James K. DrennenEmail author
Article

Abstract

This article is the first of a series of articles detailing the development of near-infrared (NIR) methods for solid-dosage form analysis. Experiments were conducted at the Duquesne University Center for Pharmaceutical Technology to qualify the capabilities of instrumentation and sample handling systems, evaluate the potential effect of one source of a process signature on calibration development, and compare the utility of reflection and transmission data collection methods. A database of 572 production-scale sample spectra was used to evaluate the interbatch spectral variability of samples produced under routine manufacturing conditions. A second database of 540 spectra from samples produced under various compression conditions was analyzed to determine the feasibility of pooling spectral data acquired from samples produced at diverse scales. Instrument qualification tests were performed, and appropriate limits for instrument performance were established. To evaluate the repeatability of the sample positioning system, multiple measurements of a single tablet were collected. With the application of appropriate spectral preprocessing techniques, sample repositioning error was found to be insignificant with respect to NIR analyses of product quality attributes. Sample shielding was demonstrated to be unnecessary for transmission analyses. A process signature was identified in the reflection data. Additional tests demonstrated that the process signature was largely orthogonal to spectral variation because of hardness. Principal component analysis of the compression sample set data demonstrated the potential for quantitative model development. For the data sets studied, reflection analysis was demonstrated to be more robust than transmission analysis.

Keywords

process analytical technology near-infrared spectroscopy chemometrics tablet analysis multivariate analysis pharmaceutical analysis 

References

  1. 1.
    FDA. PAT—A Framework for Innovative Manufacturing and Quality Assurance, Draft Guidance; 2003.Google Scholar
  2. 2.
    FDA. Guidance Documents, Available at: http://www.fda.gov/cder/guidance/index.htm. Accessed June 20, 2004.Google Scholar
  3. 3.
    Norris KH, Butler WL. Techniques for obtaining absorption spectra on intact biological samples.IRE transactions on bio-medical electronics. July 1961;8:153–157.CrossRefGoogle Scholar
  4. 4.
    Williams P, Norris K, eds.Near-Infrared Technology in the Agricultural and Food Industries. St. Paul, MN: American Association of Cereal Chemists; 2001.Google Scholar
  5. 5.
    Ciurczak EW, Torlini RP, Demkowicz MP.Determination of particle size of pharmaceutical raw materials using near-infrared reflectance spectroscopy.Spectroscopy. (Duluth, MN, United States). 1986;1:36–39.Google Scholar
  6. 6.
    Shah NK, Gemperline PJ. Combination of the Mahalanobis distance and residual variance pattern recognition techniques for classification of near-infrared reflectance spectra.Analytical Chemistry. 1990;62:465–470.CrossRefGoogle Scholar
  7. 7.
    El-Hagrasy AS, Morris HR, D’Amico F, Lodder RA, Drennen JK 3rd. Near-infrared spectroscopy and imaging for the monitoring of powder blend homogeneity.J Pharm Sci. 2001;90:1298–1307.CrossRefGoogle Scholar
  8. 8.
    Sekulic SS, Wakeman J, Doherty P, Hailey PA. Automated system for the on-line monitoring of powder blending processes using near-infrared spectroscopy. Part II. Qualitative approaches to blend evaluation.J Pharm Biomed Anal. 1998;17:1285–1309.CrossRefGoogle Scholar
  9. 9.
    Wargo DJ, Drennen JK. Near-infrared spectroscopic characterization of pharmaceutical powder blends.Journal of Pharmaceutical and Biomedical Analysis. 1996;14:1415–1423.CrossRefGoogle Scholar
  10. 10.
    Rantanen J, Antikainen O, Mannermaa J-P, Yliruusi J. Use of the near-infrared reflectance method for measurement of moisture content during granulation.Pharmaceutical Development and Technology. 2000;5:209–217.CrossRefGoogle Scholar
  11. 11.
    Rantanen J, Jørgensen A, Räsänen E, et al. Process analysis of fluidized bed granulation.AAPS PharmSciTech. 2001;2:21.CrossRefGoogle Scholar
  12. 12.
    Bijlani VJ, Delado-Lopez M, Adeyeye CM, Drennen JK. Near infrared spectroscopy for monitoring the hardness of roller compaction ribbons.NIR news. 2002;13:8–14.Google Scholar
  13. 13.
    Morris KR, Stowell JG, Byrn SR, Placette AW, Davis TD, Peck GE. Accelerated fluid bed drying using NIR monitoring and phenomenological modeling.Drug Development and Industrial Pharmacy. 2000;26:985–988.CrossRefGoogle Scholar
  14. 14.
    Ciurczak EW, James K, Drennen I.Pharmaceutical and Medical Applications of Near-Infrared Spectroscopy. New York, NY: Marcel Dekker Inc; 2002.Google Scholar
  15. 15.
    Ciurczak EW. Growth of near-infrared spectroscopy in pharmaceutical and medical sciences. In: DJ Bornhop, DA Dunn, RP Mariella Jr, CJ Murphy, DV Nicolau, S Nie, M Palmer, R Raghavachari, eds. Proceedings of SPIE Volume: 4626. Bellingham, WA: SPIE; 2002:116–125.CrossRefGoogle Scholar
  16. 16.
    Brown SD, Sum ST, Despagne F, Lavine BK. Chemometrics.Analytical Chemistry. 1996;68:21–61.CrossRefGoogle Scholar
  17. 17.
    Mobley PR, Kowalski BR, Workman JJ Jr, Bro R. Review of Chemometrics Applied to Spectroscopy: 1985–95, Part 2.Applied Spectroscopy Reviews. 1996;31:347–368.CrossRefGoogle Scholar
  18. 18.
    Workman JJ Jr, Mobley PR, Kowalski BR, Bro R. Review of chemometrics applied to spectroscopy: 1985–95, Part I.Applied Spectroscopy Reviews. 1996;31:73–124.CrossRefGoogle Scholar
  19. 19.
    Drennen JK, Lodder RA. Nondestructive near-infrared analysis of intact tablets for determination of degradation products.Journal of Pharmaceutical Sciences. 1990;79:622–627.CrossRefGoogle Scholar
  20. 20.
    Iyer M, Morris HR, Drennen JK III. Solid dosage form analysis by near infrared spectroscopy: Comparison of reflectance and transmittance measurements including the determination of effective sample mass.Journal of Near Infrared Spectroscopy. 2002;10:233–245.Google Scholar
  21. 21.
    Kirsch JD, Drennen JK. Determination of film-coated tablet parameters by near-infrared spectroscopy.J Pharm Biomed Anal. 1995;13:1273–1281.CrossRefGoogle Scholar
  22. 22.
    Kirsch JD, Drennen JK. Near-infrared spectroscopy: applications in the analysis of tablets and solid pharmaceutical dosage forms.Appl Spectr Rev. 1995;30:139–174.CrossRefGoogle Scholar
  23. 23.
    Kirsch JD, Drennen JK. Nondestructive tablet hardness testing by near-infrared spectroscopy: a new and robust spectral best-fit algorithm.J Pharm Biomed Anal. 1999;19:351–362.CrossRefGoogle Scholar
  24. 24.
    Ingle JD, Crouch SR.Spectrochemical Analysis. Upper Saddle River, NJ: Prentice-Hall; 1988.Google Scholar
  25. 25.
    United States Pharmacopeial Convention I. [1119] Near-Infrared Spectrophotometry.USP-NF, Second Supplement. Rockville, MD USA: United States Pharmacopeial Convention Inc; 2003;3337–3344.Google Scholar
  26. 26.
    Cogdill RP, Anderson CA, Drennen JK. Process Analytical Technology Case Study, Part III: Calibration Monitoring and Transfer.AAPS PharmSciTech. 2005; In press.Google Scholar
  27. 27.
    Sparen A, Malm M, Josefson M, Folestad S, Johansson J. Light leakage effects with different sample holder geometries in quantitative near-infrared transmission spectroscopy of pharmaceutical tablets.Applied Spectroscopy. 2002;56:586–592.CrossRefGoogle Scholar
  28. 28.
    ASTM.International Standard E2363-04 Standard Terminology Relating to Process Analytical Technology in the Pharmaceutical Industry; 2004.Google Scholar
  29. 29.
    Cogdill RP, Anderson CA, Delgado-Lopez M, et al. Process Analytical Technology Case Study, Part II: Development and Validation of Quantitative for Tablet API Content and Hardness.AAPS PharmSciTech. 2005;E273–E283.Google Scholar
  30. 30.
    AACC. “Near-Infrared Methods: Guidelines for Model Development and Maintenance,” AACC Method 39-00.Approved Methods of the American Association of Cereal Chemists. 10 ed. St. Paul, MN: AACC Press; 1999.Google Scholar

Copyright information

© American Association of Pharmaceutical Scientists 2005

Authors and Affiliations

  • Robert P. Cogdill
    • 1
  • Carl A. Anderson
    • 1
  • Miriam Delgado-Lopez
    • 1
  • David Molseed
    • 1
  • Robert Chisholm
    • 2
  • Raymond Bolton
    • 2
  • Thorsten Herkert
    • 3
  • Ali M. Afnán
    • 4
  • James K. Drennen
    • 1
    Email author
  1. 1.Duquesne University Center for Pharmaceutical TechnologyPittsburgh
  2. 2.AstraZenecaMacclesfieldUK
  3. 3.AstraZeneca GmbHPlankstadtGermany
  4. 4.Center for Drug Evaluation and Research, Office of Pharmaceutical ScienceUS Food and Drug AdministrationRockville

Personalised recommendations