Table III: Phenylephrine (PE)–HCl repeatability.
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The Vision software has a routine-analysis method for calculating CU automatically and produces a report that complies with
21 CFR Part 11. Table IV shows the CU results for 4.0 mg CPM in T-5 label claim tablets. Data out of the ±15% of label-claim range
because of processing difficulties are in red. Table V shows the CU results for 10.0 mg PE–HCl in the same tablets.
Table IV: Content uniformity of chlorpheniramine maleate. Relative standard deviation = 4.573%.
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Table VI shows the HPLC data in percent of label claim for the nominal label claim of batch T-5. The mean value for CPM (target
label claim of 4.0 mg) was extremely low because of formulation and tablet-processing problems. While the variance (i.e.,
RSD) was not more than 6.0 % in the T-5 values, T-3 for PE–HCL was 6.26%, and T-9 for CPM was 6.68% (see Table VI).
Conclusion
Table V: Content uniformity of phenylephrine–HCl. Relative standard deviation = 1.627%.
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This study shows that the NIR assay for the determination of tablets' CU is a fast and accurate means of monitoring tablets
that could be used for production and is consistent with FDA's PAT initiative. The data showed promising results that could
relieve laboratory workload and bring analysis closer to real time for process monitoring. Ten tablets could be analyzed in
less than 3 min. The results would be improved by eliminating processing problems that led to high within-batch variance (i.e.,
as high as 11.95% RSD in N-1 CPM) and meeting target label-claim values.
Table VI: High-performance liquid chromatography data for percent of nominal label claims and batch levels tablets. Data out
of the ±15% of label claim range and relative standard deviations above 6.0% are in red.
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Robert Mattes* is an applications scientist, and Denise Root is the marketing and product specialist manager, both at FOSS NIRSystems, 7703 Montpelier Rd., Laurel, MD 20723, tel. 301.680.7251,
fax 301.236.0134, rmattes@foss-nirsystems.com
. Ed Brunson is an instructor of pharmaceutical sciences, Suresh Potharaju is a graduate student, Wen Qu is a research associate, James Johnson is an associate professor of pharmaceutics, and Hassan Almoazen is an assistant professor of pharmaceutics, all at the University of Tennessee Health Science Center.
*To whom all correspondence should be addressed.
Submitted: July 18, 2011. Accepted: Sept. 26, 2011.
References
1. J. Workman, Jr., Handbook of Near-Infrared Analysis, D.A. Burns and E.W. Ciuczak, Eds. (Marcel Dekker, New York, 2nd ed., 2001), p. 94.
2. K.R. Beebe, R.J. Pell, and M.B. Seasholtz, Chemometrics: A Practical Guide, (John Wiley and Sons, Hoboken, NJ, 1998), p. 1.
3. FDA, PAT: A Framework for Innovative Pharmaceutical Development, Manufacturing, and Quality Assurance (Rockville, MD, Sept. 2004).
4. R. Mattes et al., Pharm. Technol.
31 (4), 170–182 (2007).
5. P.J. Larkin, E. Fruhling, and C. Longfellow, Am. Pharm. Rev.
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6. R. Kramer, Chemometric Techniques for Quantitative Analysis, (Marcel Dekker, New York, 1998), p. 60.
7. J. Workman, Jr. and L. Weyer, Practical Guide to Interpretive Near-Infrared Spectroscopy, (CRC Press, Boca Raton, FL, 2008), p. 43.
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