13C solid-state NMR analysis of the most common pharmaceutical excipients used in solid drug formulations, Part I: Chemical shifts assignment

• 13C CP/MAS NMR spectra of the most common pharmaceutical excipients are presented.
• All signals in the solid-state NMR spectra were assigned with discussion of chemical shifts.
• GIPAW calculations were employed for the crystalline excipients.
• Summary of the ssNMR data on excipients is useful in drug analysis and design

Solid-state NMR is an excellent and useful method for analyzing solid-state forms of drugs. In the 13C CP/MAS NMR spectra of the solid dosage forms many of the signals originate from the excipients and should be distinguished from those of active pharmaceutical ingredient (API). In this work the most common pharmaceutical excipients used in the solid drug formulations: anhydrous α-lactose, α-lactose monohydrate, mannitol, sucrose, sorbitol, sodium starch glycolate type A and B, starch of different origin, microcrystalline cellulose, hypromellose, ethylcellulose, methylcellulose, hydroxyethylcellulose, sodium alginate, magnesium stearate, sodium laurilsulfate and Kollidon® were analyzed. Their 13C CP/MAS NMR spectra were recorded and the signals were assigned, employing the results (R2: 0.948–0.998) of GIPAW calculations and theoretical chemical shifts. The 13C ssNMR spectra for some of the studied excipients have not been published before while for the other signals in the spectra they were not properly assigned or the assignments were not correct. The results summarize and complement the data on the 13C ssNMR analysis of the most common pharmaceutical excipients and are essential for further NMR studies of API-excipient interactions in the pharmaceutical formulations.

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