title: ¹³C solid-state NMR analysis of the most common pharmaceutical excipients used in solid drug formulations, Part I: Chemical shifts assignment.
abstract: Solid-state NMR is an excellent and useful method for analyzing solid-state forms of drugs. In the (13)C 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 (13)C CP/MAS NMR spectra were recorded and the signals were assigned, employing the results (R(2): 0.948-0.998) of GIPAW calculations and theoretical chemical shifts. The (13)C 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 (13)C ssNMR analysis of the most common pharmaceutical excipients and are essential for further NMR studies of API-excipient interactions in the pharmaceutical formulations.
authors: Faculty of Pharmacy, Medical University of Warsaw, Department of Physical Chemistry, Banacha 1, 02-093 Warsaw, Poland. Electronic address: dpisklak@wum.edu.pl.
authors: Dariusz Maciej
authors: DM
authors: Pisklak
authors: Faculty of Pharmacy, Medical University of Warsaw, Department of Inorganic and Analytical Chemistry, Banacha 1, 02-093 Warsaw, Poland.
authors: Monika Agnieszka
authors: MA
authors: Zielińska-Pisklak
authors: Faculty of Pharmacy, Medical University of Warsaw, Department of Physical Chemistry, Banacha 1, 02-093 Warsaw, Poland.
authors: Łukasz
authors: Ł
authors: Szeleszczuk
authors: Faculty of Pharmacy, Medical University of Warsaw, Department of Physical Chemistry, Banacha 1, 02-093 Warsaw, Poland.
authors: Iwona
authors: I
authors: Wawer
mesh_terms: D066241:Carbon-13 Magnetic Resonance Spectroscopy / Q000379:methods*; D002626:Chemistry, Pharmaceutical / Q000379:methods; D005079:Excipients / Q000737:chemistry*; D004364:Pharmaceutical Preparations / Q000737:chemistry*
chemical_list: D005079:Excipients; D004364:Pharmaceutical Preparations
keywords: Excipients; GIPAW; Solid drug forms; Solid state NMR