Detection of acetylcodeine in urine as an indicator of illicit heroin use:Method validation and results of a pilot study

Background: Acetylcodeine (AC), an impurity of illicit heroin synthesis, ha s been suggested as an interesting biomarker of illicit heroin use. Methods: Procedures were developed for quantification of (a) morphine, 6-mo noacetylmorphine (6-AM), and codeine in urine and (b) diacetylmorphine and AC in urine. Solid-phase extraction of the analytes was performed, and the extracted analytes were analyzed by selected-ion monitoring with gas chroma tography-mass spectrometry. This procedure required prior derivatization wi th propionic anhydride. Results: Different validation parameters were determined, such as linearity , reproducibility, extraction recoveries, and cutoffs. Seventy-one urine sp ecimens of illicit heroin abusers and 44 urine specimens of subjects in a h eroin maintenance program were analyzed. AC was detected in 85.9% of the sa mples of the first group but not in any of the samples from subjects taking medical heroin. In the two groups, there were 94.4% and 84.1% 6-AM positiv e urine specimens, respectively. Detection times were determined for AC and codeine by parallel administration of heroin containing various percentage s of AC to four voluntary patients in a heroin maintenance program. The mea sured detection times were 8 and 23 h for AC and codeine, respectively. Conclusions: These results indicate that, together with detection of 6-AM i n urine, AC is a suitable marker of illicit heroin use. (C) 2001 American A ssociation for Clinical Chemistry.