Determination of Nofedone in Human Serum by Electron-Capture GLC

Abstract

An electron-capture GLC method to measure nofedone in human serum was developed. A homolog of nofedone was added to the serum as an internal standard before the sample was alkalinized with pH 9.5 phosphate buffer and extracted with ethylene dichloride containing 0.5% isopentyl alcohol. This organic phase was extracted with 0.2 N HCl, the acidic aqueous phase was neutralized immediately, and the extraction with ethylene dichloride was repeated. The ethylene dichloride phase was evaporated to dryness, and the residue was reacted with heptafluorobutyric anhydride. The derivatives were chromatographed at 290° on a 1% Dexsil 300 column. Data on apparent recovery, accuracy, and specificity are given. The detection limit was 5ng/ml of serum. Serum levels over time in one patient after intravenous administration of 1mg/kg and after oral administration of 50, 100, and 150mg of nofedone are presented.