Trace analysis of Azo bis (isobutyronitrile) in pharmaceuticals by capillary gas chromatography with flame ionization detection

K.Rama Seshaiah, Sudip Kr.Sama

Abstract

A capillary gas chromatographic method using flame ionization detection was developed and validated for the trace analysis (ppm level) of Azo bis (isobutyronitrile) in pharmaceutical drug substance. The method utilizes a megabore capillary column with 5% Phenyl-95%methylpolysiloxane stationary phase.Adissolve-and-injection approachwas adopted for sample introduction in a split mode (1:1). Methanol is used as sample solvent. A limit of detection of about 0.5ppmand limit of quantitation of about 1.8ppm were achieved for theAzo bis (isobutyronitrile) in drug substance samples. The method optimization and validation are also discussed in this paper.