Pharmaceutical Research

, Volume 25, Issue 5, pp 1100–1109

The USP Performance Verification Test, Part I: USP Lot P Prednisone Tablets—Quality Attributes and Experimental Variables Contributing to Dissolution Variance

  • Gang Deng
  • Alyssa J. Ashley
  • William E. Brown
  • Joseph W. Eaton
  • Walter W. Hauck
  • Loice C. Kikwai
  • Mark R. Liddell
  • Ronald G. Manning
  • Jimmy M. Munoz
  • Pallavi Nithyanandan
  • Maria J. Glasgow
  • Erika Stippler
  • Samir Z. Wahab
  • Roger L. Williams
Research Paper

Abstract

Purpose

Beyond instrumental qualification, proficiency testing is not usually a prerequisite for many analytical procedures, given reliance on a manufacturer’s assay validation coupled with regulatory review and inspection. Given the special features of the dissolution procedure, proficiency testing was put in place initially by pharmaceutical manufacturers and carried on by USP. Proficiency testing is designed to help ensure that execution of a dissolution procedure for solid oral dosage forms adequately supports administrative and legal decisions so that measurements made at different times, by different analysts, or with different methods can be confidently compared. USP has applied metrological principles to aid practitioners in carrying out the dissolution procedure alone and in collaborative studies to facilitate understanding potential sources of variability.

Materials and Methods

The present study aimed to identify key dissolution variables associated with USP Lot P Prednisone Tablets in conjunction with the USP Performance Verification Test (PVT). Using five dissolution test assemblies from different manufacturers, at least four of six analysts determined percents prednisone dissolved on dissolution Apparatus 1 (basket) and Apparatus 2 (paddle) on each assembly. Six replicate experiments were performed on each analyst–assembly combination with a set of six to eight tablets in each experiment.

Results and Conclusions

Statistical analysis demonstrated that dissolution test assemblies were the largest factor contributing to dissolution variability. Inherent tablet variability was low, and USP Lot P Prednisone Tablets did not contribute importantly to dissolution variability. Contributions from analyst and analytical procedure also were estimated to be low.

Key words

dissolution performance verification performance verification test quality assurance United States Pharmacopeia 

References

  1. 1.
    USP, USP 30–NF 25, Dissolution <711>, United States Pharmacopeial Convention, Inc., Rockville, MD, 2001, pp. 277–282.Google Scholar
  2. 2.
    W. W. Hauck, T. Foster, E. Sheinin, T. L. Cecil, W. Brown, M. Marques, and R. L. Williams. Oral dosage form performance tests: new dissolution approaches. Pharm. Res 22:182–187 (2005).PubMedCrossRefGoogle Scholar
  3. 3.
    FDA, Center for Drug Evaluation and Research. Guidance for industry: waiver of in vivo bioavailability and bioequivalence studies for immediate-release solid oral dosage forms based on a biopharmaceutics classification system. (2000). www.fda.gov/cder/guidance/3618fnl.pdf. Accessed October 19, 2007.
  4. 4.
    WHO. 2005. Multisource (generic) pharmaceutical products: guidelines on registration requirements to establish interchangeability. Geneva, Switzerland: WHO. (2005). www.who.int/medicines/services/expertcommittees/pharmprep/QAS04_093Rev4_final.pdf. Accessed October 19, 2007.
  5. 5.
    M. Glasgow, S. Dressman, W. Brown, T. Foster, S. Schuber S, R. G. Manning, S. Z. Wahab, R. L. Williams, and W. W. Hauck W. W. The USP performance verification test, part II: collaborative study of USP’s Lot P Prednisone Tablets. DOI 10.1007/s11095-007-9482-2 (2008).
  6. 6.
    NIST. Guidance on federal conformity assessment activities. Fed. Regist. 65:48894–48902 (2000).Google Scholar
  7. 7.
    FDA. Guidance for industry: text on validation of analytical procedures. (1995). www.fda.gov/cder/guidance/ichq2a.pdf. Accessed October 19, 2007.
  8. 8.
    ISO. ISO 5725 1-6: Accuracy (Trueness and Precision) of Measurement Methods and Results. ISO, Geneva, Switzerland, 1994.Google Scholar
  9. 9.
    ISO. ISO/IEC Guide 43-1: Proficiency Testing by Interlaboratory Comparisons. ISO, Geneva, Switzerland, 1997.Google Scholar
  10. 10.
    J. Dressman, and J. Kramer. Pharmaceutical Dissolution Testing. Taylor & Francis, Boca Raton, FL, 2005.Google Scholar
  11. 11.
    R. Hanson, and V. Gray. Handbook of Dissolution Testing, 3rd ed. Dissolution Technologies, Hockessin, DE, 2004.Google Scholar
  12. 12.
    J. Eaton, G. Deng, W. W. Hauck, W. Brown, R. G. Manning, and S. Wahab. Perturbation study of dissolution apparatus variables—a design of experiment approach. Dissolution Technol. 14:20–26 (2007).Google Scholar
  13. 13.
    M. R. Liddell, G. Deng, W. W. Hauck, W. Brown, S. Wahab, and R. G. Manning. Evaluation of glass dissolution vessel dimensions and irregularities. Dissolution Technol. 14:28–33 (2007).Google Scholar
  14. 14.
    S. A. Qureshi, and I. J. McGilveray. Typical variability in drug dissolution testing: study with USP and FDA calibrator tablets and a marketed drug (glibenclamide) product. Eur. J. Pharm. Sci. 7:249–258 (1999).PubMedCrossRefGoogle Scholar
  15. 15.
    S. A. Qureshi, and J. Shabnam. Cause of high variability in drug dissolution testing and its impact on setting tolerances. Eur. J. Pharm. Sci. 12:271–276 (2001).PubMedCrossRefGoogle Scholar
  16. 16.
    Z. Gao, T. W. Moore, A. P. Smith, W. H. Doub, and B. J. Westenberger. Studies of variability in dissolution testing with USP apparatus 2. J. Pharm. Sci. 96:1794–1801 (2007).PubMedCrossRefGoogle Scholar
  17. 17.
    J. L. Baxter, J. Kukura, and F. J. Muzzio. Hydrodynamics-induced variability in the USP Apparatus 2 dissolution test. Int. J. Pharm. 292:17–29 (2005).PubMedCrossRefGoogle Scholar
  18. 18.
    J. Kukura, J. L. Baxter, and F. J. Muzzio. Shear distribution and variability in the USP apparatus 2 under turbulent conditions. Int. J. Pharm. 279:9–17 (2004).PubMedCrossRefGoogle Scholar
  19. 19.
    USP. The USP performance test: mechanical calibration vs. a periodic performance verification test with reference standard tablets (calibrators) [and links therein]. www.usp.org/USPNF/notices/calibratorsPublicStatement.html. Accessed October 19, 2007.
  20. 20.
    R. Hanson. Comments on mechanical and chemical calibration by an instrument manufacturer. Dissolution Technol. 14:7(2007).Google Scholar

Copyright information

© Springer Science+Business Media, LLC 2007

Authors and Affiliations

  • Gang Deng
    • 1
  • Alyssa J. Ashley
    • 1
  • William E. Brown
    • 1
  • Joseph W. Eaton
    • 1
  • Walter W. Hauck
    • 1
  • Loice C. Kikwai
    • 1
  • Mark R. Liddell
    • 1
  • Ronald G. Manning
    • 2
  • Jimmy M. Munoz
    • 1
  • Pallavi Nithyanandan
    • 1
  • Maria J. Glasgow
    • 1
  • Erika Stippler
    • 3
  • Samir Z. Wahab
    • 1
  • Roger L. Williams
    • 1
  1. 1.United States PharmacopeiaRockvilleUSA
  2. 2.Department of Health and Human ServicesWashingtonUSA
  3. 3.US PharmacopeiaDepartment of Reference Materials DevelopmentRockvilleUSA

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