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 c linical trials. Amylamine may be present as a trace impurity in BMS-18 1 866-02. BMS-188 494-04 is the TBA salt of the prodrug ester of BMS-1 87 745, a novel oral hypocholesterolemic agent. Chromatographic separa tions were accomplished under isocratic conditions using a Dionex CS-1 4 column with conductivity detection. The methods differ only in the c omposition of the methanesulfonic acid-acetonitrile mobile phase. The detection limit and minimum quantifiable levels for amylamine were 0.0 1% and 0.02%, respectively. The method was linear over the range studi ed (1-12.5 mu g/ml, n=7, r=0.9993). The method for TBA was linear from 5 to 30% (w/w) (50-300 mu g/ml, n=8, r=0.9993) of working sample conc entration (1 mg/ml BMS-188 494-04). The precision and accuracy of the methods are presented.