PMID- 24056058 OWN - NLM STAT- MEDLINE DCOM- 20140812 LR - 20131204 IS - 1873-3441 (Electronic) IS - 0939-6411 (Linking) VI - 85 IP - 3 Pt B DP - 2013 Nov TI - Quantitative on-line vs. off-line NIR analysis of fluidized bed drying with consideration of the spectral background. PG - 1064-74 LID - S0939-6411(13)00305-6 [pii] LID - 10.1016/j.ejpb.2013.09.012 [doi] AB - Quantitative dehydration studies of dibasic calcium phosphate anhydrous (DCPA) in a small-scale cold-model fluidized bed dryer with process air control were conducted. Near-infrared spectroscopy (NIRS) with partial least squares regression (PLSR) was used to predict DCPAs' residual moisture content. Loss-on-drying (LOD) was employed as a reference method and confirmed the actual moisture content of DCPA. First, dynamic PLSR modeling was carried out, i.e., the NIR spectra were on-line recorded and predicted throughout the drying process. Secondly, PLSR off-line modeling was performed, i.e., samples were consecutively thief-probed from the processor, put into glass vials and analyzed off-line. Furthermore, two background spectra were collected prior to the in- and off-line measurements in an attempt to increase the method's sensitivity, i.e., (i) dry DCPA that was fluidized at respective process air velocity (on-line) or inside a glass vial (off-line) and (ii) Spectralon(R)--a highly reflecting standard reference material made of fluoropolymer. Benefits and drawbacks of the in- and off-line approaches with different spectral backgrounds are discussed in detail. The results indicated that (i) the thief-probed sample amount from the processor and thus the sample weight and (ii) the downtime between thief-probing a sample and its actual analysis via NIRS and LOD can bias the moisture content predictions. CI - Copyright (c) 2013 Elsevier B.V. All rights reserved. FAU - Heigl, Nicolas AU - Heigl N AD - Research Center Pharmaceutical Engineering, Graz, Austria. FAU - Koller, Daniel M AU - Koller DM FAU - Glasser, Benjamin J AU - Glasser BJ FAU - Muzzio, Fernando J AU - Muzzio FJ FAU - Khinast, Johannes G AU - Khinast JG LA - eng PT - Journal Article DEP - 20130918 PL - Netherlands TA - Eur J Pharm Biopharm JT - European journal of pharmaceutics and biopharmaceutics : official journal of Arbeitsgemeinschaft fur Pharmazeutische Verfahrenstechnik e.V JID - 9109778 RN - 0 (Buffers) RN - 0 (Calcium Phosphates) RN - 0 (Excipients) RN - 059QF0KO0R (Water) RN - 9011-14-7 (Polymethyl Methacrylate) RN - 97Z1WI3NDX (calcium phosphate) SB - IM MH - Air MH - Buffers MH - Calcium Phosphates/*chemistry MH - Calibration MH - Chemistry, Pharmaceutical/methods MH - Excipients/chemistry MH - Least-Squares Analysis MH - Multivariate Analysis MH - Polymethyl Methacrylate/chemistry MH - Reference Values MH - Reproducibility of Results MH - Software MH - Spectroscopy, Near-Infrared/*methods MH - Technology, Pharmaceutical/*instrumentation/methods MH - Temperature MH - Time Factors MH - Water/chemistry OTO - NOTNLM OT - Dibasic calcium phosphate anhydrous OT - Fluidized bed OT - Near-infrared spectroscopy OT - Off-line OT - On-line OT - Partial least squares regression OT - Spectral background EDAT- 2013/09/24 06:00 MHDA- 2014/08/13 06:00 CRDT- 2013/09/24 06:00 PHST- 2012/12/07 00:00 [received] PHST- 2013/08/23 00:00 [revised] PHST- 2013/09/11 00:00 [accepted] PHST- 2013/09/24 06:00 [entrez] PHST- 2013/09/24 06:00 [pubmed] PHST- 2014/08/13 06:00 [medline] AID - S0939-6411(13)00305-6 [pii] AID - 10.1016/j.ejpb.2013.09.012 [doi] PST - ppublish SO - Eur J Pharm Biopharm. 2013 Nov;85(3 Pt B):1064-74. doi: 10.1016/j.ejpb.2013.09.012. Epub 2013 Sep 18.