Format

Send to

Choose Destination
AAPS J. 2015 Nov;17(6):1501-10. doi: 10.1208/s12248-015-9806-9. Epub 2015 Aug 25.

2D-Cosy NMR Spectroscopy as a Quantitative Tool in Biological Matrix: Application to Cyclodextrins.

Author information

1
CHU, Laboratory of Pharmaceutical Technology and Biopharmacy, Department of Pharmacy, University of Liege, Tower 4, 2nd floor, Avenue de l'hôpital,1, 4000, Liège, Belgium. gilles.dufour@ulg.ac.be.
2
CHU, Laboratory of Pharmaceutical Technology and Biopharmacy, Department of Pharmacy, University of Liege, Tower 4, 2nd floor, Avenue de l'hôpital,1, 4000, Liège, Belgium.
3
Laboratory of Medicinal Chemistry, Department of Pharmacy, Center for Interdisciplinary Research on Medicines (CIRM), University of Liege, 4000, Liège, Belgium.

Abstract

Classical analytical quantifications in biological matrices require time-consuming sample pre-treatments and extractions. Nuclear magnetic resonance (NMR) analysis does not require heavy sample treatments or extractions which therefore increases its accuracy in quantification. In this study, even if quantitative (q)NMR could not be applied to 2D spectra, we demonstrated that cross-correlations and diagonal peak intensities have a linear relationship with the analyzed pharmaceutical compound concentration. This work presents the validation process of a 2D-correlation spectroscopy (COSY) NMR quantification of 2-hydroxypropyl-β-cyclodextrin in plasma. Specificity, linearity, precision (repeatability and intermediate precision), trueness, limits of quantification (LOQs), and accuracy were used as validation criteria. 2D-NMR could therefore be used as a valuable and accurate analytical technique for the quantification of pharmaceutical compounds, including hardly detectable compounds such as cyclodextrins or poloxamers, in complex biological matrices based on a calibration curve approach.

KEYWORDS:

2D-NMR; biological matrices; cyclodextrins; poloxamers; quantification

PMID:
26304859
PMCID:
PMC4627452
DOI:
10.1208/s12248-015-9806-9
[Indexed for MEDLINE]
Free PMC Article

Supplemental Content

Full text links

Icon for Springer Icon for PubMed Central
Loading ...
Support Center