Analytical method for piperazine in an active pharmaceutical ingredient using chemical derivatization and HPLC-UV

R. Navaneeswari and P. Raveend

Abstract

A method to form a UV-active derivative of piperazine was developed. The method was based on the reaction of piperazine with NBD-Cl (4-chloro-7-nitrobenzofuran), forming a stable derivative, which was UV-active. The method was used to analyze samples of an active pharmaceutical ingredient (API) for trace amounts of Piperazine. The derivatization approach allowed detection of piperazine at low levels, using readily available HPLC-UV instrumentation. The method was validated with respect to Limit of detection, Limit of quantification, Accuracy, linearity, precision, robust and ruggedness in the range of about 30 to 350 ppm. It was shown through spiked recovery tests that the derivatization reaction occurred smoothly without interference from the API.