Ion chromatography of amylamine and tert.-butylamine in pharmaceuticals.
Ion chromatographic (IC) methods have been developed for the assay of amylamine in BMS-181 866-02 and tert.-butylamine (TBA) in BMS-188 494-04. BMS-181 866-02 is the penultimate intermediate in the synthesis of a novel thromboxane antagonist, BMS-180 291-02, which is undergoing clinical trials. Amylamine may be present as a trace impurity in BMS-181 866-02. BMS-188 494-04 is the TBA salt of the prodrug ester of BMS-187 745, a novel oral hypocholesterolemic agent. Chromatographic separations were accomplished under isocratic conditions using a Dionex CS-14 column with conductivity detection. The methods differ only in the composition of the methanesulfonic acid-acetonitrile mobile phase. The detection limit and minimum quantifiable levels for amylamine were 0.01% and 0.02%, respectively. The method was linear over the range studied (1-12.5 micrograms/ml, n = 7, r = 0.9993). The method for TBA was linear from 5 to 30% (w/w) (50-300 micrograms/ml, n = 8, r = 0.9993) of working sample concentration (1 mg/ml BMS-188 494-04). The precision and accuracy of the methods are presented.
Jagota
N K
NK
Analytical R&D, Bristol-Myers Squibb, Pharmaceutical Research Institute, New Brunswick, NJ 08903-0191, USA.
Chetram
A J
AJ
Nair
J B
JB
D000588:Amines / Q000032:analysis*; D002082:Butylamines / Q000032:analysis*; D002845:Chromatography / Q000379:methods*; D004340:Drug Contamination; D004364:Pharmaceutical Preparations / Q000032:analysis*; D012680:Sensitivity and Specificity; D013451:Sulfonic Acids
D000588:Amines; C103126:BMS 181866-02; C103127:BMS 188494-04; D002082:Butylamines; D004364:Pharmaceutical Preparations; D013451:Sulfonic Acids; C025397:tert-butylamine; C005264:n-amylamine