LC determination of dinitrosopiperazine in simulated gastric juice

A simple and specific reversed phase HPLC method for the determination of d initrosopiperazine in simulated gastric juice using UV detection was report ed. The chromatographic resolution of the analyte and the internal standard isosorbide dinitrate was performed without extraction from the gastric jui ce on a reversed phase ODS column, Isocratic elution was carried out with m ethanol-0.02 M sodium dihydrogen phosphate (60:40 v/v, pH 3.0) at a flow ra te of 1.0 ml min(-1) with UV detection at 238 nm. The calibration graph was linear over the concentration range 0.072-2.88 mug ml(-1) of dinitrosopipe razine with minimum detectability (S/N = 2) of 0.01 mug ml(-1) (8 x 10(-8) M). Inter-day and intra-day precisions calculated as% RSD were in the range 0.32-0.38% and 0.19-0.25% respectively. Inter-day and intra-day accuracies calculated as% error were in the range 0.18-0.21 and 0.08-0.11% respective ly. The proposed method was successfully applied to the study of the possib le in-vivo production of DNPZ under the standard nitrosation conditions rec ommended by WHO. (C) 2001 Elsevier Science B.V. All rights reserved.