Browse > Article
http://dx.doi.org/10.17480/psk.2016.60.2.85

Online Real-Time Monitoring of Moisture in Pharmaceutical Granules During Fluidized Bed Drying Using Near-Infrared Spectroscopy  

Kim, Jaejin (Chong Kun Dang Pharm.)
Kim, Byung-Suk (Chong Kun Dang Pharm.)
Lim, Young-Il (Chong Kun Dang Pharm.)
Woo, Young-Ah (Chong Kun Dang Pharm.)
Publication Information
YAKHAK HOEJI / v.60, no.2, 2016 , pp. 85-91 More about this Journal
Abstract
Drying of granules for tablet formulation is one of the important unit operations. The loss on drying method is traditionally used for this purpose. However, it is a time-consuming method, requiring at least 1 h. Moreover, it is ineffective in monitoring the moisture content of granules during the drying process. In this study, online real-time monitoring of moisture content during the drying process was successfully performed using near-infrared (NIR) spectroscopy. NIR spectra were collected during 15 different drying batches for developing a reliable NIR spectroscopic method. Such a large number of batches were used to develop a more robust partial least squares (PLS) model. NIR spectra collected from 12 batches were used for developing the model that was validated by predicting the moisture content of the samples in the remaining 3 batches. The standard errors of predictions (SEPs) in the measurement of batch 1, batch 2, and batch 3 were 0.52%, 0.57%, and 0.56%, respectively. The online NIR spectroscopic method developed in this study was reliable and accurate in monitoring the moisture content during the drying process.
Keywords
drying process; near-infrared spectroscopy; Process Analytical Technologies (PAT); real-time monitoring; fluidized bed drying;
Citations & Related Records
연도 인용수 순위
  • Reference
1 USFDA, Guidance for industry: PAT - A framework for innovative pharmaceutical development, manufacturing and quality assurance (2004).
2 ICH, Validation of Analytical Procedures: Text and Methodology Q2 (R1) (1994).
3 Wang, H. G., Senior, P. R., Mann, R. and Yang, W. Q. : Online measurement and control of solids moisture in fluidized bed dryers. Chem. Eng. Sci. 64, 2893 (2009).   DOI
4 Buschmüller, C., Wiedey, W., Döscher, C., Dressler, J. and Breitkreutz, J. : In-line monitoring of granule moisture in fluidized-bed dryers using microwave resonance technology. Eur. J. Pharm. Biopharm. 69, 380 (2008).   DOI
5 Fonteyne, M., Gildemyn, D., Peeters, E., Mortier, S. T., Vercruysse, J., Gernaey, K. V., Vervaet, C., Remon, J. P., Nopens, I. and Beer, T. D. : Moisture and drug solid-state monitoring during a continuous drying process using empirical and mass balance models. Eur. J. Pharm. Biopharm. 87, 616 (2014).   DOI
6 Findlay, W. P., Peck, G. R. and Morris, K. R. : Determination of fluidized bed granulation end point using near-infrared spectroscopy and phenomenological analysis. J. Pharm. Sci. 94, 604 (2005).   DOI
7 Green, R. L., Thurau, G. T., Pixley, N. C., Mateos, A., Reed, R. A. and Higgins, P. : In-line monitoring of moisture content in fluid bed dryers using near-ir spectroscopy with consideration of sampling effects on method accuracy. Anal. Chem. 77, 4515 (2005).   DOI
8 Märk, J., Karner, M., Andre, M., Rueland, J. and Huck, C. W. : Online process control of a pharmaceutical intermediate in a fluidized-bed drier environment using near-infrared spectroscopy. Anal. Chem. 82, 4209 (2010).   DOI
9 Kim, J., Han, J., Noh, J. and Chung, H. : Feasibility of a wide area illumination scheme for reliable raman measurement of petroleum products. Appl. Spectrosc. 61, 686 (2007).   DOI
10 우영아, 조창희, 김효진, 조정환, 조경규, 정승성, 김수정, 김중환 : 근적외선 분광법을 이용한 생약의 원산지 판별. 약학회지 42, 359 (1998).
11 Kim, J., Hwang, J. and Chung, H. : Comparison of near-infrared and raman spectroscopy for on-line monitoring of etchant solutions directly through a teflon tube. Anal. Chim. Acta 629, 119 (2008).   DOI
12 Yoon, J., Kim, J., Duy, P. K., Kim, M., Kang, S. and Chung, H. : Diffuser-incorporated transmission NIR measurement for reliable analysis of packed granular samples. Analyst 138, 4922 (2013).   DOI
13 Watano, S., Terashita, K. and Miyanami, K. : Determination of end-point with a complex granulation applying infrared moisture sensor. Chem. Pharm. Bull. 39, 1013 (1991).   DOI
14 Nieuwmeyer, F. J. S., Damen, M., Gerich, A., Rusmini, F., Maarschalk, K. V. and Vromans, H. : Granule characterization during fluid bed drying by development of a near infrared method to determine water content and median granule size. Pharm. Res. 24, 1854 (2007).   DOI
15 Peinado, A., Hammond, J. and Scott, A. : Development, validation and transfer of a near infrared method to determine in-line the end point of a fluidised drying process for commercial production batches of an approved oral solid dose pharmaceutical product. J. Pharm. Biomed. Anal. 54, 13 (2011).   DOI
16 Fonteyne, M., Arruabarrena, J., Beer, J. D., Hellings, M., Kerkhof, T. V. D., Burggraeve, A., Vervaet, C., Remon, J. P. and Beer, T. D. : NIR spectroscopic method for the in-line moisture assessment during drying in a six-segmented fluid bed dryer of a continuous tablet production line: validation of quantifying abilities and uncertainty assessment. J. Pharm. Biomed. Anal. 100, 21 (2014).   DOI