title: Improved solid-state NMR quantifications of active principles in pharmaceutical formulations.
abstract: The facility of implementation reached by solid-state nuclear magnetic resonance (ssNMR) spectroscopy makes this technique increasingly popular in pharmaceutical sciences, and more specifically for the dosage of active principles in pharmaceutical formulations, since about 80% of the formulations currently available on the market are present in the solid form. In this case, analysis by MAS NMR allows faster and simplified protocols, as a solubilization step is not required. However, the specificity of the ssNMR experiments should be explicitly taken into account when designing an accurate measurement procedure. In this work we show that, by using a combination of external concentration referencing and a properly designed sample preparation optimized for quantitative determinations, quantification of active principles in pharmaceutical formulations can be performed with both speed and precision. The method is illustrated by reinvestigating the dosage of Meprobamate, an anxiolytic agent typically prescribed in case of anxiety or muscular soreness, present in a commercial formulation (Equanil). Specifically, with respect to previously proposed analytical protocols, the procedure outlined here allows fast quantification with excellent precision.
authors.affiliation: Aix-Marseille Université, ISM2-UMR-6263, Equipe CES, case 512, av. Escadrille Normandie Niémen, 13397 Marseille Cedex 20, France.
authors.forename: Stéphanie
authors.initials: S
authors.lastname: Sanchez
authors.forename: Fabio
authors.initials: F
authors.lastname: Ziarelli
authors.forename: Stéphane
authors.initials: S
authors.lastname: Viel
authors.forename: Corinne
authors.initials: C
authors.lastname: Delaurent
authors.forename: Stefano
authors.initials: S
authors.lastname: Caldarelli
mesh_terms: D014151:Anti-Anxiety Agents / Q000032:analysis* / Q000737:chemistry; D002247:Carbon Isotopes; D002626:Chemistry, Pharmaceutical; D004304:Dosage Forms; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008620:Meprobamate / Q000032:analysis* / Q000737:chemistry; D015394:Molecular Structure; D004364:Pharmaceutical Preparations; D012015:Reference Standards; D013678:Technology, Pharmaceutical; D013997:Time Factors
chemical_list: D014151:Anti-Anxiety Agents; D002247:Carbon Isotopes; D004304:Dosage Forms; D004364:Pharmaceutical Preparations; D008620:Meprobamate