Skip to main content
SpringerLink
Log in

Assessment of NIR spectroscopy for nondestructive analysis of physical and chemical attributes of sulfamethazine bolus dosage forms

  • Published:
AAPS PharmSciTech Aims and scope Submit manuscript

Abstract

The goal of this study was to assess the utility of near infrared (NIR) spectroscopy for the determination of content uniformity, tablet crushing strength (tablet hardness), and dissolution rate in sulfamethazine veterinary bolus dosage forms. A formulation containing sulfamethazine, corn starch, and magnesium stearate was employed. The formulations were wet granulated with a 10% (wt/vol) starch paste in a high shear granulator and dried at 60°C in a convection tray dryer. The tablets were compressed on a Stokes B2 rotary tablet press running at 30 rpm. Each sample was scanned in reflectance mode in the wavelengths of the NIR region. Principal component analysis (PCA) of the NIR tablet spectra and the neat raw materials indicated that the scores of the first 2 principal components were highly correlated with the chemical and physical attributes. Based on the PCA model, the significant wavelengths for sulfamethazine are 1514, (1660–1694), 2000, 2050, 2150, 2175, 2225, and 2275 nm; for corn starch are 1974, 2100, and 2325 nm; and for magnesium stearate are 2325 and 2375 nm. In addition, the loadings show large negative peaks around the water band regions (≈1420 and 1940 nm), indicating that the partial least squares (PLS) models could be affected by product water content. A simple linear regression model was able to predict content uniformity with a correlation coefficient of 0.986 at 1656 nm; the use of a PLS regression model, with 3 factors, had anr 2 of 0.9496 and a sandard error of calibration of 0.0316. The PLS validation set had anr 2 of 0.9662 and a standard error of 0.0354. PLS calibration models, based on tablet absorbance data, could successfully predict tablet crushing strength and dissolution in spite of varying active pharmaceutical ingredient (API) levels. Prediction plots based on these PLS models yielded correlation coefficients of 0.84 and 0.92 on independent validation sets for crushing strength and Q120 (percentage dissolved in 120 minutes), respectively.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. Ritchie GE, Roller RW, Ciurczak EW, Mark H, Tso C, MacDonald SA. Validation of a near-infrared transmission spectroscopic procedure Part B: Application to alternate content uniformity and release assay methods for pharmaceutical solid dosage forms.J Pharm Biomed Anal. 2002;29:159–171.

    Article  CAS  Google Scholar 

  2. Candolfi A, De Maesschalck R, Massart DL, Hailey PA, Harrington AC. Identification of pharmaceutical excipients using NIR spectroscopy and SIMCA.J Pharm Biomed Anal. 1999;19:923–935.

    Article  CAS  Google Scholar 

  3. Ulmschneider M, Pénigault E. Direct identification of key intermediates in containers using Fourier-transform near-infrared spectroscopy through the protective polyethylene primary packaging.Analysis. 2000;28:136–140.

    Article  CAS  Google Scholar 

  4. Otsuka M, Katol F, Matsuda Y, Ozaki Y. Comparative determination of polymorphs of indomethacin in powders and tablets by chemometrical near-infrared spectroscopy and X-ray powder diffractometry.AAPS Pharm Sci Tech. 2003;4:E19.

    Article  Google Scholar 

  5. Buckton G, Yonemochi E, Yoon WL, Moffat AC. Water sorption and near IR spectroscopy to study the differences between microcrystalline cellulose and silicified microcrystalline cellulose before and after wet granulation.Int J Pharm. 1999;181:41–47.

    Article  CAS  Google Scholar 

  6. Rantanen J, Rasanen E, Tenhunen J, Kansakoski M, Mannermaa J, Yliruusi J. In-line moisture measurement during granulation with a four-wavelength near infrared sensor: evaluation of particle size and binder effects.Eur J Pharm Biopharm. 2000;50:271–276.

    Article  CAS  Google Scholar 

  7. Lodder RA, Selby M, Hieftje gM. Detection of capsule tampering by near-infrared reflectance analysis.Anal Chem. 1987;59:1921–1930.

    Article  CAS  Google Scholar 

  8. Derbyshire HM, Feldman Y, Bland CR, Broadhead J, Smith G. A study of the molecular properties of water in hydrated mannitol.J Pharm Sci. 2002;91:1080–1088.

    Article  CAS  Google Scholar 

  9. Drennen JK, Lodder RA. Nondestructive near-infrared analysis of intact tablets for determination of degradation products.J Pharm Sci. 1990;79:622–627.

    Article  CAS  Google Scholar 

  10. Gustafsson C, Nystroem C, Lennholm H, Bonferoni MC, Caramella CM. Characteristics of hydroxypropyl methylcellulose influencing compactibility and prediction of particle and tablet properties by infrared spectroscopy.J Pharm Sci. 2003;92:494–504.

    Article  CAS  Google Scholar 

  11. Kuny T, Schatz C, Ulmschneider M, Marrer S, Leuenberger H. Non-destructive dissolution testing correlation.Dissolution Technologies. 2003;10:22–28.

    CAS  Google Scholar 

  12. Morisseau KM, Rhodes CT. Near-infrared spectroscopy as a nondestructive alternative to conventional tablet hardness testing.Pharm Res. 1997;14:108–111.

    Article  CAS  Google Scholar 

  13. Reich G. Potential of attenuated total reflection infrared and near-infrared spectroscopic imaging for quality assurance/quality control of solid pharmaceutical dosage forms.Pharm Ind. 2002;64:870–874.

    CAS  Google Scholar 

  14. Otsuka M, Mouri Y, Matsuda Y. Chemometric evaluation of pharmaceutical properties of antipyrine granulates by near-infrared spectroscopy.AAPS PharmSciTech. 2003;4:E47.

    Article  Google Scholar 

  15. Higgins JP, Arrivo SM, Thurau G, et al. Spectroscopic approach for on-line monitoring of particle size during the processing of pharmaceutical nanoparticles.Anal Chem. 2003;75:1777–1785.

    Article  CAS  Google Scholar 

  16. Fahmy R, Marnane W, Bensley D, Hollenbeck G. Dissolution testing of veterinary products.Dissolution Technologies. 2001;8:8–14.

    CAS  Google Scholar 

  17. Du J, Hoag SW. Characterization of excipient and tableting factors that influence folic acid dissolution, friability and breaking strength of oil- and water-soluble multivitamin with minerals tablets.Drug Dev Ind Pharm. 2003;29:1137–1147.

    Article  CAS  Google Scholar 

  18. Kramer R.Chemometric Techniques for Quantitative Analysis. New York, NY: Marcel Dekker Inc; 1998.

    Google Scholar 

  19. Brereton RG. Chemometrics Data Analysis for the Laboratory and Chemical Plant. Chichester, UK: John Wiley & Sons Ltd; 2003.

    Google Scholar 

  20. Otto M. Chemometrics Statistics and Computer Application in Analytical Chemistry. Weinheim, Germany: Wiley-VCH; 1999.

    Google Scholar 

  21. Wu H, Lyon RC, Hussain AS, et al. Application of principal component analysis in assessing pharmaceutical formulation design: exploring the causal links between the tablet processing conditions and drug dissolution rate. AICHE Topical Conference: Discovery, Development, and Delivery of Medicines. AICHE Annual Meeting: November: 17–19, 2003: San Francisco, CA:635–642.

  22. Beebe KR, Pell RJ, Seasholtz MB.Chemometrics: A Practical Guide. New York, NY: John Wiley & Sons Inc; 1998.

    Google Scholar 

Download references

Author information

Authors and Affiliations

  1. School of Pharmacy, University of Maryland-Baltimore, 20 N Pine St, 21201, Baltimore, Maryland

    Aditya S. Tatavarti, Gary Hollenbeck & Stephen W. Hoag

  2. Office of New Animal Drug Evaluation, Center for Veterinary Medicine, US Food and Drug Administration, 20855, Rockville, MD

    Raafat Fahmy, William Marnane & Dennis Bensley

  3. Office of Pharmaceutical Science, Center for Drug Evaluation and Research, US Food and Drug Administration, 20852, Rockville, MD

    Huiquan Wu & Ajaz S. Hussain

Authors
  1. Aditya S. Tatavarti
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Raafat Fahmy
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Huiquan Wu
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Ajaz S. Hussain
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. William Marnane
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Dennis Bensley
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Gary Hollenbeck
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. Stephen W. Hoag
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Stephen W. Hoag.

Additional information

Published: September 20, 2005

The opinions expressed in this paper are of the authors' personal views. They do not necessarily reflect the views or policies of the FDA.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Tatavarti, A.S., Fahmy, R., Wu, H. et al. Assessment of NIR spectroscopy for nondestructive analysis of physical and chemical attributes of sulfamethazine bolus dosage forms. AAPS PharmSciTech 6, 15 (2005). https://doi.org/10.1208/pt060115

Download citation

  • Received:

  • Accepted:

  • DOI: https://doi.org/10.1208/pt060115

Keywords

Search

Navigation