In-line multipoint near-infrared spectroscopy for moisture content quantification during freeze-drying

A. Kauppinen (Corresponding Author), Maunu Toiviainen, O. Korhonen, J. Aaltonen, K. Järvinen, Janne Paaso, Mikko Juuti, J. Ketolainen

    Research output: Contribution to journalArticleScientificpeer-review

    38 Citations (Scopus)

    Abstract

    During the past decade, near-infrared (NIR) spectroscopy has been applied for in-line moisture content quantification during a freeze-drying process. However, NIR has been used as a single-vial technique and thus is not representative of the entire batch. This has been considered as one of the main barriers for NIR spectroscopy becoming widely used in process analytical technology (PAT) for freeze-drying. Clearly it would be essential to monitor samples that reliably represent the whole batch. The present study evaluated multipoint NIR spectroscopy for in-line moisture content quantification during a freeze-drying process. Aqueous sucrose solutions were used as model formulations. NIR data was calibrated to predict the moisture content using partial least-squares (PLS) regression with Karl Fischer titration being used as a reference method. PLS calibrations resulted in root-mean-square error of prediction (RMSEP) values lower than 0.13%. Three noncontact, diffuse reflectance NIR probe heads were positioned on the freeze-dryer shelf to measure the moisture content in a noninvasive manner, through the side of the glass vials. The results showed that the detection of unequal sublimation rates within a freeze-dryer shelf was possible with the multipoint NIR system in use. Furthermore, in-line moisture content quantification was reliable especially toward the end of the process. These findings indicate that the use of multipoint NIR spectroscopy can achieve representative quantification of moisture content and hence a drying end point determination to a desired residual moisture level.
    Original languageEnglish
    Pages (from-to)2377-2384
    Number of pages8
    JournalAnalytical Chemistry
    Volume85
    Issue number4
    DOIs
    Publication statusPublished - 2013
    MoE publication typeA1 Journal article-refereed

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