Determination of primary amines by benzenesulfonylation/GC with flame photometric detection

Abstract

A selective and sensitive method for the determination of primary amines by GC is described. After benzenesulfonylation of amines by Hinsberg reaction, primary amines were completely separated from secondary amines by extraction with hexane in 50% potassium hydroxide-22.5% methanol solution. Benzenesulfonyl derivatives of primary amines in acidic aqueous layer were extracted by diethyl ether, and analyzed by GC with flame photometric detection (FPD-GC) using a DB-1 capillary column. Derivatization yield of butylamine was 96.7±4.0% (n=3). By FPD-GC, the calibration curves of amines were linear in the range of 201000 ng for the derivatives and the detection limits were about 10100pg as injection amounts, which were above 20 times more sensitive than that obtained by GC with flame ionization detection.