Comparison of the analytical methods (solid state NMR, FT-IR, PXRD) in the analysis of the solid drug forms with low concentration of an active ingredient – 17-β-estradiol case

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Graphical abstractHighlightsVarious techniques (IR,PXRD,NMR) in the analysis of solid dosage forms were compared.Low dosage pharmaceutical formulations analysis was performed.13C solid state NMR enabled the identification of API in the formulation.The application of various techniques (FT-IR, PXRD, ssNMR) in the analysis of solid dosage forms with low concentration of an API (17-β-estradiol hemihydrate, EBHH) was tested. PXRD analysis of Estrofem Mite tablets (EMT) confirmed the presence of the main crystalline excipient, α-lactose monohydrate. In the PXRD pattern of EMT the strong background from polycrystalline excipients, i.e. hydroxypropylmethylcellulose and corn starch was observed. FT-IR spectra were characterized by the broad peaks in the 3000–3600 cm−1 region of the O—H stretching modes coming from multiple hydrogen bonds that are present in the structures of the excipients (α-lactose monohydrate, corn starch) and API. The only technique which unambiguously confirmed the presence of an API in the EMT was solid state NMR. Despite the tabletting process each of the EMT component retained its characteristic features like relaxation time and TI. Due to the possibility of the manipulation in the experimental registration parameters like recycle delay (RD), evolution time (τ) and contact time (CT) it was possible to perform multiple experiments on the same sample of EMT. The most valuable were the inversion recovery CP experiments in which, by setting the proper values of τ, it was possible to selectively observe the signals of the chosen component of the drug formulation. In this study the great potential of solid state NMR in the analysis of solid dosage forms, as the unique technique that combines the possibility of selective observation of the chosen signals with the non destructive character that enables further analysis of the same sample, was confirmed.

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