GAS-CHROMATOGRAPHIC MASS-SPECTROMETRIC QUANTITATION OF DEXTROPROPOXYPHENE AND NORPROPOXYPHENE IN HAIR AND WHOLE-BLOOD AFTER AUTOMATED ONLINE SOLID-PHASE EXTRACTION - APPLICATION IN 12 FATALITIES

After conversion of norpropoxyphene (NP) to its corresponding amide, d extropropoxyphene (DP) and NP are extracted from 1 ml of blood or 50 m g of powdered hair, on C-18 cartridges and eluted using methanol conta ining 0.5% acetic acid. Automated extraction is conducted on-line with automated device, starting from buffered and centrifuged sample. Afte r extraction, the dried residue is reconstituted with 40 mu l of metha nol, and then injected in a gas chromatograph at 250 degrees C. Quanti tation is carried out by gas chromatography-mass spectrometry in the s elected-ion monitoring mode, lidocaine being the internal standard. Th e method gave relative standard deviations lower than 6.2% in whole bl ood, and 6.0% in hair for the entire range of calibration from 0.5 to 10 mu g/ml in blood and from 1 to 20 ng/mg in hair of both compounds. Limits of detection in blood and hair for DP are, respectively, 0.07 m u g/ml and 0.05 ng/mg, whereas the respective limits of detection in w hole blood and hair for NP are 0.09 mu g/ml and 0.04 ng/mg. The presen t method was used for one year in our laboratory. Postmortem concentra tions of DP in blood ranged from 1.6 to 44.0 mu g/ml (mean=9.8 mu g/ml , n=12) and are comparable to those found in the literature. Out of 30 hair samples from people who died from heroin overdose, 13 were posit ive both for DP and NP with concentrations ranging from 0.2 to 27.4 ng /mg (mean 8.7 ng/mg) for DP and 0.3 to 68.9 ng/mg (mean 24.1 ng/mg) fo r NP. (C) 1998 Elsevier Science B.V.