Raman spectroscopy and capillary zone electrophoresis for the analysis of degradation processes in commercial effervescent tablets containing acetylsalicylic acid and ascorbic acid.

In order to ensure the stability of pharmaceutical products appropriate manufacturing and storage conditions are required. In general, the degradation of active pharmaceutical ingredients (APIs) and subsequent formation of degradation products affect the pharmaceutical quality. Thus, a fast and effective detection and characterization of these substances is mandatory. Here, the applicability of Raman spectroscopy and CZE for the characterization of the degradation of effervescent tablets containing acetylsalicylic acid (ASA) and ascorbic acid (AA) was evaluated. Therefore, a degradation study was performed analyzing tablets from two different manufacturers at varying conditions (relative humidity (RH) 33%, 52% and 75% at 30°C). Raman spectroscopy combined with principal component analysis could be successfully applied for the fast and easy discrimination of non-degraded and degraded effervescent tablets after a storage period of approximately 24h (RH 52%). Nevertheless, a clear identification or quantification of APIs and degradation products within the analyzed tablets was not possible, i.a. due to missing reference materials. CZE-UV enabled the quantification of the APIs (ASA, AA) and related degradation products (salicylic acid (SA); semi-quantitative also mono- and diacetylated AA) within the complex tablet mixtures. The higher the RH, the faster the degradation of ASA and AA as well as the formation of the degradation products. Mono- and diacetylated AA are major primary degradation products of AA for the applied effervescent tablets. A significant degradation of the APIs was detected earlier by CZE (6-12h, RH 52%) than by Raman spectroscopy. Summarized, Raman spectroscopy is well-suited as quick test to detect degradation of these tablets and CZE can be utilized for further detailed characterization and quantification of specific APIs and related degradation products.

Neuberger S ，Jooß K ，Flottmann D ，Scriba G ，Neusüß C ... -  《-》

Quantification of ascorbic acid and acetylsalicylic acid in effervescent tablets by CZE-UV and identification of related degradation products by heart-cut CZE-CZE-MS.

Neuberger S ，Jooß K ，Ressel C ，Neusüß C ... -  《-》

Determination of counterfeit medicines by Raman spectroscopy: Systematic study based on a large set of model tablets.

In the last decade, counterfeit pharmaceutical products have become a widespread issue for public health. Raman spectroscopy which is easy, non-destructive and information-rich is particularly suitable as screening method for fast characterization of chemicals and pharmaceuticals. Combined with chemometric techniques, it provides a powerful tool for the analysis and determination of counterfeit medicines. Here, for the first time, a systematic study of the benefits and limitations of Raman spectroscopy for the analysis of pharmaceutical samples on a large set of model tablets, varying with respect to chemical and physical properties, was performed. To discriminate between the different mixtures, a combination of dispersive Raman spectroscopy performing in backscattering mode and principal component analysis was used. The discrimination between samples with different coatings, a varying amount of active pharmaceutical ingredients and a diversity of excipients were possible. However, it was not possible to distinguish between variations of the press power, mixing quality and granulation. As a showcase, the change in Raman signals of commercial acetylsalicylic acid effervescent tablets due to five different storage conditions was monitored. It was possible to detect early small chemical changes caused by inappropriate storage conditions. These results demonstrate that Raman spectroscopy combined with multivariate data analysis provides a powerful methodology for the fast and easy characterization of genuine and counterfeit medicines.

Neuberger S ，Neusüß C 《-》

Assay of effervescent tablets by near-infrared spectroscopy in transmittance and reflectance mode: acetylsalicylic acid in mono and combination formulations.

Merckle P ，Kovar KA 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》

Comparative study of the continuous wavelet transform, derivative and partial least squares methods applied to the overlapping spectra for the simultaneous quantitative resolution of ascorbic acid and acetylsalicylic acid in effervescent tablets.

Dinç E ，Ozdemir A ，Baleanu D 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》