Quantitation and determination of molecular weight distribution of residual water soluble extractable polyamines in DMP 504, a poly-alkylamine bile acid sequestrant, by aqueous high performance size exclusion chromatography.
A high performance size exclusion chromatography (HPSEC) method with refractive index detection for quantitation and molecular weight determination of extractable water soluble polyamines (SPA) in a novel proprietary polymeric pharmaceutical compound (DMP 504) is described. The extracted polyamines are synthetic impurities as well as potential degradation products of the polymer. Data for calibration, precision, solution stability, and limits of detection and quantitation are presented to validate the suitability of this method for its intended purpose. Response linearity for the poly(2-vinylpyridine) standard is demonstrated between 10 and 1000 micrograms ml-1, equivalent to 0.005% and 0.5% (w/w) in DMP 504. Molecular weight distributions of SPA extracted from DMP 504 are presented. No increase in SPA is detected in DMP 504 over 6 months storage at room temperature.
Juliano
K
K
Pharmaceutical Research and Development, DuPont Merck Pharmaceutical Company, Wilmington, DE 19880, USA.
Champion
W L
WL
Schreiber
M A
MA
Blackwell
J A
JA
D002138:Calibration; D002850:Chromatography, Gel; D008970:Molecular Weight; D011073:Polyamines / Q000032:analysis; D011108:Polymers / Q000032:analysis*; D000644:Quaternary Ammonium Compounds / Q000032:analysis*; D012996:Solutions
C111415:DMP-504; D011073:Polyamines; D011108:Polymers; D000644:Quaternary Ammonium Compounds; D012996:Solutions