title: A simplified procedure for the determination of free codeine, free morphine, and 6-acetylmorphine in urine.
abstract: A procedure for detection and quantification of free codeine, free morphine, and 6-acetylmorphine in urine is presented. The analytes were extracted at neutral pH by solid-phase extraction prior to derivatization to their trifluoroacetyl derivatives. The derivatized extracts were analyzed by gas chromatography/mass spectrometry in the electron impact mode. Confirmation of the analytes was accomplished by comparing the ion abundance ratios of the analytes to those of a previously analyzed standard. The qualitative ion abundance ratios were required to be within 20% of those of the standard for acceptance. Quantification was based on the tri-deuterated analogs of the analytes. Linearity was obtained in the range of 10 to 1000 ng/mL, with correlation coefficients of all analytes exceeding 0.999. Percent recoveries were 90% for codeine, 88% for morphine, and 85% for 6-acetylmorphine. No hydrolysis of 6-acetylmorphine occurs during the extraction procedure. The authors also studied the stability of 6-acetylmorphine at various storage conditions of pH, temperature, and chemical preservation. 6-Acetylmorphine was found to be stable for 12 weeks when stored at -17 degrees C.
authors.affiliation: Sierra Nevada Laboratories Inc., Reno, Nevada 89502.
authors.forename: D C
authors.initials: DC
authors.lastname: Fuller
authors.forename: W H
authors.initials: WH
authors.lastname: Anderson
mesh_terms: D002623:Chemistry Techniques, Analytical / Q000379:methods; D003061:Codeine / Q000652:urine*; D004355:Drug Stability; D004356:Drug Storage; D006801:Humans; D006863:Hydrogen-Ion Concentration; D006868:Hydrolysis; D009020:Morphine / Q000652:urine*; D009022:Morphine Derivatives / Q000652:urine*; D015203:Reproducibility of Results; D015813:Substance Abuse Detection / Q000379:methods*; D013696:Temperature
chemical_list: D009022:Morphine Derivatives; D009020:Morphine; C026979:6-O-monoacetylmorphine; D003061:Codeine