Development and validation of an in-line NIR spectroscopic method for continuous blend potency determination in the feed frame of a tablet press

De Leersnyder, F.; Peeters, E.; Djalabi, H.; Vanhoorne, V.; Van Snick, B.; Hong, K.; Hammond, S.; Liu, A. Y.; Ziemons, Eric; Vervaet, C.; De Beer, T.

doi:10.1016/j.jpba.2018.01.032

Article (Scientific journals)

Development and validation of an in-line NIR spectroscopic method for continuous blend potency determination in the feed frame of a tablet press

De Leersnyder, F.; Peeters, E.; Djalabi, H. et al.

2018 • In Journal of Pharmaceutical and Biomedical Analysis, 151, p. 274-283

Peer Reviewed verified by ORBi

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https://hdl.handle.net/2268/220678

DOI
10.1016/j.jpba.2018.01.032

PubMed
29413975

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Keywords :

Accuracy profiles; Feed frame; In-line NIR spectroscopy; Partial least squares; Process analytical technology; Rotary tablet press

Abstract :

[en] A calibration model for in-line API quantification based on near infrared (NIR) spectra collection during tableting in the tablet press feed frame was developed and validated. First, the measurement set-up was optimised and the effect of filling degree of the feed frame on the NIR spectra was investigated. Secondly, a predictive API quantification model was developed and validated by calculating the accuracy profile based on the analysis results of validation experiments. Furthermore, based on the data of the accuracy profile, the measurement uncertainty was determined. Finally, the robustness of the API quantification model was evaluated. An NIR probe (SentroPAT FO) was implemented into the feed frame of a rotary tablet press (Modul™ P) to monitor physical mixtures of a model API (sodium saccharine) and excipients with two different API target concentrations: 5 and 20% (w/w). Cutting notches into the paddle wheel fingers did avoid disturbances of the NIR signal caused by the rotating paddle wheel fingers and hence allowed better and more complete feed frame monitoring. The effect of the design of the notched paddle wheel fingers was also investigated and elucidated that straight paddle wheel fingers did cause less variation in NIR signal compared to curved paddle wheel fingers. The filling degree of the feed frame was reflected in the raw NIR spectra. Several different calibration models for the prediction of the API content were developed, based on the use of single spectra or averaged spectra, and using partial least squares (PLS) regression or ratio models. These predictive models were then evaluated and validated by processing physical mixtures with different API concentrations not used in the calibration models (validation set). The β-expectation tolerance intervals were calculated for each model and for each of the validated API concentration levels (β was set at 95%). PLS models showed the best predictive performance. For each examined saccharine concentration range (i.e., between 4.5 and 6.5% and between 15 and 25%), at least 95% of future measurements will not deviate more than 15% from the true value. © 2018

Research Center/Unit :

CIRM - Centre Interdisciplinaire de Recherche sur le Médicament - ULiège

Disciplines :

Pharmacy, pharmacology & toxicology

Author, co-author :

De Leersnyder, F.; Laboratory Process Analytical Technology, Department of Pharmaceutics, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium

Peeters, E.; Pfizer > SPECTech Group, Analytical R&D

Djalabi, H.; Laboratory Process Analytical Technology, Department of Pharmaceutics, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium

Vanhoorne, V.; Laboratory of Pharmaceutical Technology, Department of Pharmaceutics, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium

Van Snick, B.; Laboratory of Pharmaceutical Technology, Department of Pharmaceutics, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium

Hong, K.; Advanced Manufacturing Technology Group, Pfizer Global Supply, Pfizer Inc., 100 US-206, Peapack, United States

Hammond, S.; Process Analytical Sciences Group, Pfizer Global Supply, Pfizer Inc., 100 US-206, Peapack, United States

Liu, A. Y.; SPECTech Group, Analytical R&D, Worldwide Research and Development, Pfizer Inc., 280 Shennecossett Rd, Groton, United States

Ziemons, Eric ; Université de Liège - ULiège > Département de pharmacie > Département de pharmacie

Vervaet, C.; Laboratory of Pharmaceutical Technology, Department of Pharmaceutics, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium

De Beer, T.; Laboratory Process Analytical Technology, Department of Pharmaceutics, Ghent University, Ottergemsesteenweg 460, Ghent, Belgium

Language :

English

Title :

Development and validation of an in-line NIR spectroscopic method for continuous blend potency determination in the feed frame of a tablet press

Publication date :

17 January 2018

Journal title :

Journal of Pharmaceutical and Biomedical Analysis

ISSN :

0731-7085

eISSN :

1873-264X

Publisher :

Elsevier

Volume :

151

Pages :

274-283

Peer reviewed :

Peer Reviewed verified by ORBi

Available on ORBi :

since 23 February 2018

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