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Transmission Low-Frequency Raman Spectroscopy for Quantification of Crystalline Polymorphs in Pharmaceutical Tablets
摘要： The purpose of this study was to quantify polymorphs of active pharmaceutical ingredients in pharmaceutical tablets using a novel transmission low-frequency Raman spectroscopy method. We developed a novel transmission geometry for low-frequency Raman spectroscopy and compared quantitative ability in transmission mode versus backscattering mode using chemometrics. We prepared two series of tablets: 1) containing different weight-based contents of carbamazepine form III and 2) including different ratios of carbamazepine polymorphs (forms I/ III). From the relationship between the contents of carbamazepine form III and partial least squares (PLS) predictions in the tablets, correlation coefficients in transmission mode (R2= 0.98) were found to be higher than in backscattering mode (R2= 0.97). The root mean square error of cross-validation (RMSECV) of the transmission mode was 3.9 compared to 4.9 for the backscattering mode. The tablets containing a mixture of carbamazepine (I/ III) polymorphs were measured by transmission low-frequency Raman spectroscopy, and it was found that the spectral shape changed according to the ratio of polymorphs: the relationship between the actual content and the prediction showed high correlation. These findings indicate that transmission low-frequency Raman spectroscopy possess the potential to complement existing analytical methods for the quantification of polymorphs.
关键词： Transmission,Carbamazepine,Pharmaceutical Tablets,Quantification,Low-Frequency Raman Spectroscopy,THz-Raman,Crystalline Polymorph
更新于2025-09-23 15:23:52
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Assembly of graphene on Ag3PO4/AgI for effective degradation of carbamazepine under Visible-light irradiation: Mechanism and degradation pathways
摘要： A highly efficient visible-light-driven photocatalyst Ag3PO4/AgI-Graphene (Ag3PO4/AgI-G) was synthesized through a chemical coprecipitation procedure. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were performed to study the physicochemical structural of the photocatalysts. The photocatalytic activity of the samples was examined by the carbamazepine (CBZ) degradation under artificial visible light and natural sunlight irradiation. Experimental results indicated that the introduction of low mass content of graphene enhanced the photocatalytic performance of Ag3PO4/AgI, and the photocatalytic degradation efficiency of CBZ over Ag3PO4/AgI-3%G (mass ratio of graphene : Ag3PO4/AgI = 3:100) reached 93.06% within 21 min, which was much higher than that over pure Ag3PO4 (26.92%) and Ag3PO4/AgI (74.38%). UV-vis diffuse reflectance spectra, photoluminescence (PL) spectra, transient photocurrent responses and electrochemical impedance spectra (EIS) of the samples were conducted to verify the high photocatalytic performance of the Ag3PO4/AgI-3%G. In addition, possible photocatalytic degradation pathways of CBZ were proposed based on the analysis of transformation products during the reaction. The reactive species trapping experiments and Electron spin resonance (ESR) analysis demonstrated that h+ and ·O2- were the main active oxidant species responsible for CBZ photodegradation. The photocatalytic degradation mechanism of CBZ over Ag3PO4/AgI-3%G under visible light irradiation was schematically proposed. This study not only provides a new technique for the synthesis of Ag3PO4-based photocatalysts with high photocatalytic activity, but also demonstrates that the Ag3PO4/AgI-3%G composite could be a promising photocatalyst for the treatment of waters containing CBZ.
关键词： Photocatalytic degradation,Carbamazepine,Z-scheme,Graphene,Ag3PO4/AgI,Visible light
更新于2025-09-23 15:21:21