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    Fiber-array-based Raman hyperspectral imaging for simultaneous chemical selective monitoring of particle size and shape of active ingredients in analgesic tablets
    (Basel : MDPI, 2019) Frosch, Timea; Wyrwich, Elisabeth; Yan, Di; Popp, Jürgen; Frosch, Torsten
    The particle shape, size and distribution of active pharmaceutical ingredients (API) are relevant quality indicators of pharmaceutical tablets due to their high impact on the manufacturing process. Furthermore, the bioavailability of the APIs from the dosage form depends largely on these characteristics. Routinely, particle size and shape are only analyzed in the powder form, without regard to the effect of the formulation procedure on the particle characteristics. The monitoring of these parameters improves the understanding of the process; therefore, higher quality and better control over the biopharmaceutical profile can be ensured. A new fiber-array-based Raman hyperspectral imaging technique is presented for direct simultaneous in-situ monitoring of three different active pharmaceutical ingredients- acetylsalicylic acid, acetaminophen and caffeine- in analgesic tablets. This novel method enables a chemically selective, noninvasive assessment of the distribution of the active ingredients down to 1 µm spatial resolution. The occurrence of spherical and needle-like particles, as well as agglomerations and the respective particle size ranges, were rapidly determined for two commercially available analgesic tablet types. Subtle differences were observed in comparison between these two tablets. Higher amounts of acetaminophen were visible, more needle-shaped and bigger acetylsalicylic acid particles, and a higher incidence of bigger agglomerations were found in one of the analgesic tablets.
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    Application of Thermal Response Measurements to Investigate Enhanced Water Adsorption Kinetics in Ball-Milled C2N-Type Materials
    (Weinheim : Wiley-VCH-Verl., 2022) Du, Shengjun; Leistenschneider, Desirée; Xiao, Jing; Dellith, Jan; Troschke, Erik; Oschatz, Martin
    Sorption-based water capture is an attractive solution to provide potable water in arid regions. Heteroatom-decorated microporous carbons with hydrophilic character are promising candidates for water adsorption at low humidity, but the strong affinity between the polar carbon pore walls and water molecules can hinder the water transport within the narrow pore system. To reduce the limitations of mass transfer, C2N-type carbon materials obtained from the thermal condensation of a molecular hexaazatriphenylene-hexacarbonitrile (HAT-CN) precursor were treated mechanochemically via ball milling. Scanning electron microscopy as well as static light scattering reveal that large pristine C2N-type particles were split up to a smaller size after ball milling, thus increasing the pore accessibility which consequently leads to faster occupation of the water vapor adsorption sites. The major aim of this work is to demonstrate the applicability of thermal response measurements to track these enhanced kinetics of water adsorption. The adsorption rate constant of a C2N material condensed at 700 °C remarkably increased from 0.026 s−1 to 0.036 s−1 upon ball milling, while maintaining remarkably high water vapor capacity. This work confirms the advantages of small particle sizes in ultramicroporous materials on their vapor adsorption kinetics. It is demonstrated that thermal response measurements are a valuable and time-saving method to investigate water adsorption kinetics, capacities, and cycling stability.