Predicting granule size distribution of a fluidized bed spray granulation process by regime based PLS modeling of acoustic emission data

Abstract Granule size distribution (GSD) is generally regarded as one of the most critical quality-affecting attributes of a fluidized bed spray granulation process. Several process analytical techniques have been applied for in- and on-line monitoring of the GSD during the process. In this study, an acoustic emission technique was used for off-line prediction of the GSD. Acoustic spectra were recorded during 24 batch fluidized bed spray granulations. An off-line analysis of the acoustic spectra was performed using partial least squares regression (PLSR). First, the acoustic data from the spraying phase was divided into separate regimes, each corresponding to distinctive physico-chemical conditions occurring during different stages of the process. Then, a synthetic calibration set was used to build, predictive models for GSD. The GSD could be predicted with good accuracy and precision. In addition, the option for using the acoustic emission technique as an early-warning system to detect process deviations was evaluated.

[1]  Jukka Rantanen,et al.  New perspectives for visual characterization of pharmaceutical solids. , 2004, Journal of pharmaceutical sciences.

[2]  M. Kaufman,et al.  Wettability of pharmaceutical solids: its measurement and influence on wet granulation , 2002 .

[3]  Javier Villa Briongos,et al.  Fluidised bed dynamics diagnosis from measurements of low-frequency out-bed passive acoustic emissions , 2006 .

[4]  Julie Varley,et al.  The uses of passive measurement of acoustic emissions from chemical engineering processes , 2001 .

[5]  Anders Berglund,et al.  PCA and PLS with very large data sets , 2005, Comput. Stat. Data Anal..

[6]  Mehrdji Hemati,et al.  Fluidized bed coating and granulation: influence of process-related variables and physicochemical properties on the growth kinetics , 2003 .

[7]  Frantisek Stepanek,et al.  The effect of primary particle surface energy on agglomeration rate in fluidised bed wet granulation , 2008 .

[8]  J. Rantanen,et al.  Use of in-line near-infrared spectroscopy in combination with chemometrics for improved understanding of pharmaceutical processes. , 2005, Analytical chemistry.

[9]  B. J. Ennis,et al.  A microlevel-based characterization of granulation phenomena , 1991 .

[10]  Theodora Kourti,et al.  Application of latent variable methods to process control and multivariate statistical process control in industry , 2005 .

[11]  A. W. Vreman,et al.  A basic population balance model for fluid bed spray granulation , 2009 .

[12]  Jingdai Wang,et al.  Study of the power spectrum of acoustic emission (AE) by accelerometers in fluidized beds , 2007 .

[13]  Denita Winstead,et al.  Study growth kinetics in fluidized bed granulation with at-line FBRM. , 2008, International journal of pharmaceutics.

[14]  James D. Litster,et al.  Growth regime map for liquid-bound granules , 1998 .

[15]  Rodolfo Pinal,et al.  Monitoring of High-shear Granulation using Acoustic Emission: Predicting Granule Properties , 2008, Journal of Pharmaceutical Innovation.

[16]  Jouko Yliruusi,et al.  Gaining fluid bed process understanding by in-line particle size analysis. , 2009, Journal of pharmaceutical sciences.

[17]  Torben Schæfer,et al.  A REVIEW ON PHARMACEUTICAL WET-GRANULATION , 1987 .

[18]  S. Iveson,et al.  Limitations of one-dimensional population balance models of wet granulation processes☆ , 2002 .

[19]  Rasmus Bro,et al.  Some common misunderstandings in chemometrics , 2010 .

[20]  Antti Poso,et al.  Estimation of granule size distribution for batch fluidized bed granulation process using acoustic emission and N‐way PLS , 2010 .

[21]  Vincent Girard,et al.  Granule breakage phenomena in a high shear mixer; influence of process and formulation variables and consequences on granule homogeneity , 2003 .

[22]  J. Rantanen,et al.  In-line moisture measurement during granulation with a four-wavelength near infrared sensor: an evaluation of particle size and binder effects. , 2000, European journal of pharmaceutics and biopharmaceutics : official journal of Arbeitsgemeinschaft fur Pharmazeutische Verfahrenstechnik e.V.

[23]  Jouko Yliruusi,et al.  Novel description of a design space for fluidised bed granulation. , 2007, International journal of pharmaceutics.

[24]  Francis J. Doyle,et al.  A three-dimensional population balance model of granulation with a mechanistic representation of the nucleation and aggregation phenomena , 2008 .

[25]  Kinetics of iron ore sinter feed granulation , 1990 .

[26]  P. Frake,et al.  Process control and end-point determination of a fluid bed granulation by application of near infra-red spectroscopy , 1997 .

[27]  James D. Litster,et al.  Growth regime map for liquid-bound granules: further development and experimental validation , 2001 .

[28]  David Bolton The Computation of Equivalent Potential Temperature , 1980 .

[29]  Satoru Watano,et al.  Direct control of wet granulation processes by image processing system , 2001 .

[30]  J. Macgregor,et al.  Monitoring batch processes using multiway principal component analysis , 1994 .

[31]  Gavin K. Reynolds,et al.  Kinetic models for granule nucleation by the immersion mechanism , 2009 .

[32]  O. Antikainen,et al.  Controlling granule size by granulation liquid feed pulsing. , 2008, International journal of pharmaceutics.

[33]  J. Rantanen,et al.  On-line monitoring of moisture content in an instrumented fluidized bed granulator with a multi-channel NIR moisture sensor , 1998 .

[34]  Cedric Briens,et al.  Use of triboelectric probes for on-line monitoring of liquid concentration in wet gas–solid fluidized beds , 2005 .

[35]  Kei Miyanami,et al.  Image processing for on-line monitoring of granule size distribution and shape in fluidized bed granulation , 1995 .

[36]  John F. MacGregor,et al.  Using On‐Line Process Data to Improve Quality: Challenges for Statisticians * , 1997 .

[37]  Barry M. Wise,et al.  The process chemometrics approach to process monitoring and fault detection , 1995 .

[38]  O. Antikainen,et al.  Does a powder surface contain all necessary information for particle size distribution analysis? , 2002, European journal of pharmaceutical sciences : official journal of the European Federation for Pharmaceutical Sciences.

[39]  J. Rantanen,et al.  Next generation fluidized bed granulator automation , 2000, AAPS PharmSciTech.

[40]  Jarkko Ketolainen,et al.  Evolution of granule structure and drug content during fluidized bed granulation by X-ray microtomography and confocal Raman spectroscopy. , 2011, Journal of pharmaceutical sciences.

[41]  Jukka Rantanen,et al.  Identifying sources of batch to batch variation in processability , 2008 .

[42]  Cedric Briens,et al.  Continuous on-line measurement of solid moisture content during fluidized bed drying using triboelectric probes , 2008 .

[43]  Torben Schæfer,et al.  Granulation: A Review on Pharmaceutical Wet-Granulation , 1987 .

[44]  Hiroyuki Tsujimoto,et al.  Monitoring particle fluidization in a fluidized bed granulator with an acoustic emission sensor , 2000 .

[45]  P. A. Taylor,et al.  Missing data methods in PCA and PLS: Score calculations with incomplete observations , 1996 .

[46]  Kenneth R Morris,et al.  Determination of fluidized bed granulation end point using near-infrared spectroscopy and phenomenological analysis. , 2005, Journal of pharmaceutical sciences.

[47]  Kim H. Esbensen,et al.  Acoustic chemometric monitoring of an industrial granulation production process : a PAT feasibility study , 2006 .

[48]  P. Teppola,et al.  Labscale fluidized bed granulator instrumented with non-invasive process monitoring devices , 2010 .

[49]  A. McBratney,et al.  Critical review of chemometric indicators commonly used for assessing the quality of the prediction of soil attributes by NIR spectroscopy , 2010 .

[50]  J. Rantanen,et al.  In-line moisture measurement during granulation with a four-wavelength near-infrared sensor: an evaluation of process-related variables and a development of non-linear calibration model , 2001 .

[51]  Antti Poso,et al.  The feasibility of using acoustic emissions for monitoring of fluidized bed granulation , 2009 .

[52]  Vincent Gerbaud,et al.  Effect of operating conditions and physico–chemical properties on the wet granulation kinetics in high shear mixer , 2009 .