Chromatographic assay of pharmaceutical compounds under column overloading.
A HPLC assay method utilizing overloaded chromatography and dual-wavelength detection was developed for a pharmaceutical formulation containing an antibacterial (clotrimazole) and a steroid (mometasone furoate) at widely different concentrations. In order to meet the limit of quantitation (LOQ) objective of not less than 0.05% of assay concentration simultaneously for both actives in the HPLC assay method, the assay concentration of the antibacterial falls into the non-linear range of its equilibrium isotherm, but still in the linear dynamic range of an ultraviolet detector. Although the analytical column is overloaded with the antibacterial and a non-symmetric elution peak is obtained, the HPLC assay method exhibits good linearity, recovery and reproducibility.
Zhu
J
J
Analytical Development, Schering-Plough Corporation, Kenilworth, NJ 07033-0530, USA.
Coscolluella
C
C
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003022:Clotrimazole / Q000032:analysis*; D000068656:Mometasone Furoate; D011244:Pregnadienediols / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013816:Thermodynamics
D011244:Pregnadienediols; D000068656:Mometasone Furoate; D003022:Clotrimazole