HPLC DETERMINATION OF TRACE HYDRAZINE LEVELS IN PHENELZINE SULFATE DRUG SUBSTANCE

An HPLC procedure for the estimation of trace hydrazine levels in phenelzine sulfate drug substance has been developed. The hydrazine is derivatized at ambient temperature with salicylaldehyde, and the salazine derivative is measured using short wavelength UV (209 nm). The salazine is separated from unreacted salicylaldehyde and other compounds using a mobile phase consisting of 60:40 acetonitrile-water. The mobile phase was pumped at a flow rate of 1.0 mL/min through a 150 mm x 4.6 mm i.d. reverse phase column (5 μm octadecylsilane, 30% carbon loading). The limit of detection of salazine produced when hydrazine sulfate reacts with salicylaldehyde in an analytical sample was found to be equivalent to 10 ppm of hydrazine (based upon 100 mg of phenelzine sulfate). Absorbance and hydrazine concentration are linear over the range of 10–1000 ppm of hydrazine, with an r2 of 0.9998 (n=7) based on peak height. Five samples of phenelzine sulfate analyzed for hydrazine content with salicylaldehyde gave an interassay reproducibility of 2.1%. © 1990, Taylor & Francis Group, LLC. All rights reserved.