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

Pharmaceutical Hydrates Analysis—Overview of Methods and Recent Advances

“…More specifically, in terms of hydrate investigation, PXRD helps to differentiate between the hydrated and dehydrated form of the substance. This is plainly visible as a drastic change of a pattern on the diffractogram [ 38 ] ( Figure 2 ).…”

“…When choosing the appropriate one in a particular case, the attention should be paid to the qualitative and quantitative composition of the excipients in the solid dosage form, which may interrupt the analysis, as well as the API content. In a recent study [ 38 ], the performance of selected solid-state analytical methods (PXRD, FT-IR, and ssNMR) in the analysis of the solid drug forms with low concentration of an active ingredient has been compared. The authors found that the only method that unambiguously confirmed the presence of a particular solvated form of API in the studied drug was ssNMR ( Figure 7 ).…”

“… Comparison of powder X-ray diffraction (PXRD) diffractograms of 17-β-estradiol anhydrate (red) received by heating the 17-β-estradiol hemihydrate (green). Source: author’s archive, more details in [ 38 ]. …”

“… Comparison of the Fourier-transformed infrared spectroscopy (FT-IR) spectra of anhydrous estradiol (black) and estradiol hemihydrate (red). Source: author’s archive, more details in [ 38 ]. …”

“… 13 C ssNMR as a method that can be used to study the effect of dehydration temperature on the received anhydrous product form. More information in [ 38 ]. Source: author’s archive.…”