Field assessment of active ingredient quantity in pharmaceutical tablets with limited calibration of near infrared spectra: An application to ciprofloxacin tablets
Awotunde, Olatunde; Cai, Jin; Azar, Christian Gabriel Elet al.
2024 • In Journal of Pharmaceutical and Biomedical Analysis, p. 116189
NIR spectroscopy; chemometrics; machine learning; substandard medicines; predictive model transferability
Abstract :
[en] Portable near-infrared (NIR) spectrophotometers have emerged as valuable tools for identifying substandard and falsified pharmaceuticals (SFPs). Integration of these devices with chemometric and machine learning models enhances their ability to provide quantitative chemical insights. However, different NIR spectrophotometer models vary in resolution, sensitivity, and responses to environmental factors such as temperature and humidity, necessitating instrument-specific libraries that hinder the wider adoption of NIR technology. This study addresses these challenges and seeks to establish a robust approach to promote the use of NIR technology in post-market pharmaceutical analysis. We developed support vector machine and partial least squares regression models based on binary mixtures of lab-made ciprofloxacin and microcrystalline cellulose, then applied the models to ciprofloxacin dosage forms that were assayed with high performance liquid chromatography (HPLC). A receiver operating characteristic (ROC) analysis was performed to set spectrophotometer independent NIR metrics to evaluate ciprofloxacin dosage forms as “meets standard,” “needs HPLC assay,” or “fails standard.” Over 200 ciprofloxacin tablets representing 50 different brands were evaluated using spectra acquired from three types of NIR spectrophotometer with 85% of the prediction agreeing with HPLC testing. This study shows that non-brand-specific predictive models can be applied across multiple spectrophotometers for rapid screening of the conformity of pharmaceutical active ingredients to regulatory standard.
Research Center/Unit :
CIRM - Centre Interdisciplinaire de Recherche sur le Médicament - ULiège [BE]
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Awotunde, Olatunde
Cai, Jin
Azar, Christian Gabriel El
Medina, Diane
Eyolfson, Samantha I
Hayes, Kathleen
Waffo Tchounga, Christelle Ange ; Université de Liège - ULiège > Unités de recherche interfacultaires > Centre Interdisciplinaire de Recherche sur le Médicament (CIRM)
Marini Djang'Eing'A, Roland ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique ; Université de Liège - ULiège > Unités de recherche interfacultaires > Centre Interdisciplinaire de Recherche sur le Médicament (CIRM)
Ziemons, Eric ; Université de Liège - ULiège > Unités de recherche interfacultaires > Centre Interdisciplinaire de Recherche sur le Médicament (CIRM)
Sacre, Pierre-Yves ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Lieberman, Marya
Language :
English
Title :
Field assessment of active ingredient quantity in pharmaceutical tablets with limited calibration of near infrared spectra: An application to ciprofloxacin tablets
This work was supported by NSF (CMMI-1842369, OISE-1559497). Pulte Initiative, University of Notre Dame for Pamoja summer award, Lucy Institute of Data and Society, University of Notre Dame for Lucy fellowship and American Chemical Society for the Fall 2022 Pfizer Travel Award.
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