title: An accurate quantitative analysis of polymorphic content by chemometric X-ray powder diffraction.
abstract: Data from X-ray powder diffraction (XRD) were subjected to a partial least-squares regression analysis (PLS) to build a calibration model for predicting the polymorphic content of carbamazepine (CBZ). The effectiveness of the PLS method in the construction of calibration models was analyzed by a scientific approach based on a regulation vector. CBZ forms I and III were characterized by differential scanning calorimetry (DSC) and XRD. Powder mixtures of forms I and III at various ratios (0-100% w/w; form III) were subjected to XRD. Five diffraction peaks were used for the peak-area method to compare with PLS. The results obtained by PLS had a better predictive accuracy compared to those of the peak-area method. The XRD-PLS method was established as a non-destructive, non-contact way to avoid the particle orientation effect based on statistical theory.
authors.affiliation: Department of Pharmaceutics, Hoshi University, Tokyo, Japan.
authors.forename: Masafumi
authors.initials: M
authors.lastname: Suda
authors.forename: Kozo
authors.initials: K
authors.lastname: Takayama
authors.forename: Makoto
authors.initials: M
authors.lastname: Otsuka
mesh_terms: D018712:Analgesics, Non-Narcotic / Q000032:analysis*; D002138:Calibration; D002220:Carbamazepine / Q000737:chemistry*; D033362:Powder Diffraction / Q000379:methods*; D011208:Powders / Q000032:analysis; D014961:X-Ray Diffraction / Q000379:methods*
chemical_list: D018712:Analgesics, Non-Narcotic; D011208:Powders; D002220:Carbamazepine