Spectrophotometric determination of N-nitroso compounds by flow injection analysis

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Abstract
A spectrophotometric method for the determination of N-nitroso compounds by flow injection analysis, based on a denitrosation reaction with hydrogen bromide-acetic acid followed by reaction of the liberated nitrite with the Griess reagent, is described. Under the optimum reaction conditions, the detection limit for N-nitrosopyrrolidine (NPYR) was 5 × 10–8 M for a sample volume of 200 µl and the relative standard deviations (n= 9) for 1 × 10–7 and 5.4 × 10–6 M NPYR were 3.8 and 0.5%, respectively. Various other N-nitroso compounds gave a similar level of response. Phenol, sorbic acid and methanol did not interfere with the determinations, whereas piperazine interfered seriously with the determination of nitrosoproline. The sampling rate was 25 samples h–1. The method was successfully applied to the analysis of two anti-cancer drug formulations, viz., nimustine hydrochloride and 1-(2-chloroethyl)-3-(methyl-α-D-glucopyranos-6-yl)-1-nitrosourea injections.

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