Jf. Furness et al., THE DETERMINATION OF METHADONE AND METABOLITES IN HUMAN URINE BY HPLCWITH ULTRAVIOLET, AND PARTICLE-BEAM MASS-SPECTROMETRIC DETECTION, Journal of liquid chromatography, 17(20), 1994, pp. 4431-4444
Liquid chromatography coupled to Mass Spectrometry has been used to id
entify and quantitate methadone and two of its metabolites following a
normal phase separation on a cyano-phase column. Solvent extraction w
as used to recover the target compounds from urine at the optimal pH o
f 10, (recovery: 88%, methadone; 75%, 2-ethylidene-1,5-dimethyl-3,3-di
phenylpyrrolidine (EDDP). Routine analysis may be performed using UV d
etection at 290 nm. However, for greater selectivity and identificatio
n of eluates mass spectrometry is preferred. In the urine samples stud
ied the methadone/EDDP ratio varied from 1:1 to 1:10. Two samples show
ed evidence for the presence of 1,5-dimethyl-3,3-diphenplpyrrolidone (
DDP). Methadone may be detected selectively at m/z = 223 but the ion a
bundance is weak. Detection using the base peak m/z = 72 is preferred
because of the increased sensitivity it confers although selectivity o
f detection is lost.