Two-phase derivatization of amitriptyline and structurally related tertiary amines for gas chromatography with...

A new derivatization technique for tertiary amines has been developed. The amine is extracted at ambient temperature after addition of sodium iodide with methylene chloride containing an aryl chloroformate ester. By use of two new reagents, 2,4-dichlorophenyl and pentafluorophenyl chloroformate, the carbamates formed have high electron-capture response. The derivatization is rapid, often completed within 5 min. Amitriptyline was determined down to 6 ng/ml directly in a spiked plasma sample. A method for selective derivatization of a tertiary amine in the presence of the corresponding secondary amine is given.