Abstract

QUANTIFICATION OF NITROSDIBUTYLAMINE (NDBA) IMPURITY IN TETRABUTYL AMMONIUM BROMIDE BY SIMPLE AND SENSITIVE LIQUID CHROMATOGRAPHY TECHNIQUE

Sachin Sonavane*, Vishal Solse, Samadhan Kadam and Virendrasingh Pa 

ABSTRACT

Objective: Detection and control of Nitrosodibutylamine in phase transfer catalyst i.e Tetra butyl ammonium bromide which is used in many API molecules such as Tramadol, Tapentadol, Prasugrel, Rabeprazole, Crizotinib, Xathenediones and many more drugs. Nitrosoamine is an organic compound containing the group –NNO attached to two organic groups. Nitrosoamines are formed by reaction of secondary or tertiary amines with a nitrosating agent. And some of nitrosoamines are classified as probable human carcinogens. A sensitive High performance liquid chromatography (HPLC) method was developed and validated for the determination of Nitrosodibutylamine in phase transfer catalyst i.e Tetra butyl ammonium bromide. HPLC column Inertsil ODS 3V, C18, 250 mm X 4.6 mm, 5 μm particle size with ultra violet detector (UV) was used. The proposed method is specific, linear, accurate, rugged and precise. The calibration curve of Nitrosodibutylamine showed good linearity over the concentration range of 0.125 ppm to 3.74 ppm with respect to test solution concentration and the regression coefficient was 0.999 for analyte. Method had very low limit of detection (LOD) and limit of quantification (LOQ) of analyte which proves that the method is sensitive and suitable for quantification of Nitrosodibutylamine impurities at trace level.

Keywords: Tetra butyl ammonium bromide; Nitrosoamine impurity; method development and validation.