Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy
| Autor: | Jian X. Wu, Åsmund Rinnan, Morten Allesø, Peter Uhd Jepsen, Solveig Warnecke, Frans van den Berg, Søren Balling Engelsen |
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| Jazyk: | angličtina |
| Rok vydání: | 2019 |
| Předmět: |
Detection limit
Materials science Crystalline 010401 analytical chemistry Near-infrared spectroscopy Analytical chemistry Lactose 02 engineering and technology NIR 021001 nanoscience & nanotechnology 01 natural sciences 0104 chemical sciences Amorphous solid chemistry.chemical_compound Crystallinity Terahertz time domain spectroscopy (THz-TDS) chemistry Partial least squares regression Amorphous Limit of detection (LOD) 0210 nano-technology Spectroscopy Terahertz time-domain spectroscopy |
| Zdroj: | Warnecke, S, Wu, J X, Rinnan, Å, Allesø, M, van den Berg, F W J, Jepsen, P U & Engelsen, S B 2019, ' Quantifying crystalline α-lactose monohydrate in amorphous lactose using terahertz time domain spectroscopy and near infrared spectroscopy ', Vibrational Spectroscopy, vol. 102, pp. 39-46 . https://doi.org/10.1016/j.vibspec.2019.03.004 |
| DOI: | 10.1016/j.vibspec.2019.03.004 |
| Popis: | Spray-dried lactose consists of an amorphous component (10–20%) as well as the crystalline monohydrate form [ 1 ]. It is commonly used as a diluent in direct compression, mainly because of its better flow characteristics compared to pure crystalline lactose. The amorphous form is metastable and can relative easily crystallize, which will affect the functionality of the pharmaceutical product. It is therefore of interest to establish methods for non-invasive and rapid assessment of the level of crystallinity in a pharmaceutical formulation. In this study, two spectroscopic methods, near infrared (NIR) spectroscopy and terahertz time domain spectroscopy (THz-TDS), are compared for their ability to determine low levels of crystalline lactose in a mixture. The aim was to find the limit of detection and limit of quantification for the two techniques. Partial least squares (PLS) regression models were developed and the root-mean-square-error-of-cross-validation (RMSECV) for the models with full concentration range were found to be 2.91% (w/w) and 0.87% (w/w) for THz-TDS and NIR, respectively. Calibrations developed on samples containing 0–10% (w/w) crystalline material resulted in RMSECVs of 0.30% (w/w) and 0.20% (w/w) for THz-TDS and NIR, respectively, while the limits of detection were 0.80% (w/w) and 0.43% (w/w), respectively. Both instrumental techniques are thus able to quantify the content of crystalline lactose in a mixture. To select one method over the other in an industrial quality assurance setting, further includes other aspects - such as sample handling, sample size, outlier information, instrument stability, etc. In all these aspects, NIR spectroscopy currently performs better than THz-TDS. |
| Databáze: | OpenAIRE |
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