Near infrared spectroscopy; Process Analytical Technology; Liquid form; Low-dose; Validation; Acetominophen
Abstract :
[en] The aim of the present study was first to develop a robust near infrared (NIR) calibration model able to determine the acetaminophen content of a low-dose syrup formulation (2 % (w/v)). Therefore, variability sources such as production campaigns, batches, API concentration, syrup basis, operators and sample temperatures were introduced in the calibration set. A prediction model was then built using Partial Least Square (PLS) regression. First derivative followed by Standard Normal Variate (SNV) were chosen as signal pre-processing. Based on the random subsets cross validation, 4 PLS factors were selected for the prediction model. The method was then validated for an API concentration ranging from 16 to 24 mg/mL (1.6-2.4 % (w/v)) using an external validation set. The 0.26 mg/mL RMSEP suggested the global accuracy of the model. The accuracy profile obtained from the validation results, based on tolerance intervals, confirmed the adequate accuracy of the results generated by the method all over the investigated API concentration range. Finally, the NIR model was used to monitor in real time the API concentration while mixing syrups containing various amounts of API, a good agreement was found between the NIR method and the theoretical concentrations.
Research Center/Unit :
CIRM - Centre Interdisciplinaire de Recherche sur le Médicament - ULiège
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Ziemons, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Mantanus, Jérôme ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Lebrun, Pierre ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Rozet, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Evrard, Brigitte ; Université de Liège - ULiège > Département de pharmacie > Pharmacie galénique
Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Language :
English
Title :
Acetaminophen determination in low-dose pharmaceutical syrup by NIR spectroscopy
Publication date :
2010
Journal title :
Journal of Pharmaceutical and Biomedical Analysis
ISSN :
0731-7085
eISSN :
1873-264X
Publisher :
Elsevier Science, Oxford, United Kingdom
Volume :
53
Pages :
510-516
Peer reviewed :
Peer Reviewed verified by ORBi
Funders :
DGTRE - Région wallonne. Direction générale des Technologies, de la Recherche et de l'Énergie
Commentary :
E. Ziemons and J. Mantanus contributed equally to this work
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