Short column gas chromatography–mass spectrometry and principal component analysis for the identification of coeluted substances in doping control analysis

The identification of four doping control substances in an artificial mixture, using short column gas chromatography–mass spectrometry (GC–MS) analysis was examined. Two chromatographic peaks were recorded in the chromatogram, using a short capillary column (1.8 m) at an oven temperature of 180°C. The first peak was associated with a mixture of a solvent derivative and an artifact. The second one corresponded to the mixture of four control substances. Principal component analysis was applied on a selected GC–MS data set of the latter peak to determine clear full spectra of pure substances from mixture spectra. The time of GC–MS analysis was significantly reduced to less than 1 min from 30 min which is a typical GC–MS analysis time, using standard methods of doping control analysis.     

Determination of dextropropoxyphene and nordextropropoxyphene in urine by liquid chromatography-electrospray ionization mass spectrometry

Dextropropoxyphene and nordextropropoxyphene were extracted from urine samples with mixed mode solid-phase extraction cartridges. After elution and evaporation to dryness, the eluate was dissolved in mobile phase and each sample was injected in a LC-ESI-MS system. Quantification was carried out in the selected ion monitoring mode. This article shows the possibility to analyse drugs of abuse substances in urine with a single quadrupole mass spectrometer if only a thorough work-up procedure and a sufficient chromatographic separation is accomplished. In order to enhance the fragmentation of the analytes, in-source fragmentation was carried out. One fragment and the pseudomolecular ion per analyte together with chromatographic retention times were sufficient to verify that the sought compound was found in the samples. In- and between day variation was lower than 10% and the recovery was well above 90%. The analytes were quantified in the range 100-10000 ng/ml urine.